# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1201 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. J. S. Miller Department of Chemistry University of Utah 315 S. 1400 E. RM Dock Salt Lake City, UT 84112-0850 USA ; _publ_contact_author_phone '+801 585 5455' _publ_contact_author_fax '+801 581 8433' _publ_contact_author_email JSMILLER@chemistry.utah.edu _publ_requested_journal 'The Journal of the Chemical Society, Chemical Communications' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Structure and Magnetic Properties of Mn(II)[N(CN)2]2(pyrazine). An Antiferromagnet with an Interpentrating 3-D Network Structure. ; loop_ _publ_author_name _publ_author_address 'Manson, J. L.' ; Department of Chemistry University of Utah 315 S. 1400 E. RM Dock Salt Lake City, UT 84112-0850 USA ; 'Incarvito, C. D.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Rheingold, A. L.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Miller, J. S.' ; Department of Chemistry University of Utah 315 S. 1400 E. RM Dock Salt Lake City, UT 84112-0850 USA ; # 3. Results data_jsm30 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H4 Mn N8' _chemical_formula_weight 267.13 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)/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 7.3514(11) _cell_length_b 16.865(2) _cell_length_c 8.8033(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.057(2) _cell_angle_gamma 90.00 _cell_volume 1091.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1158 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description Blade _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker P4/CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3428 _diffrn_reflns_av_R_equivalents 0.0928 _diffrn_reflns_av_sigmaI/netI 0.1208 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 23.99 _reflns_number_total 1556 _reflns_number_gt 1019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 'Idealized contributions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1556 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1981 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.003 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 0.7393(3) 0.13759(10) 0.13398(17) 0.0188(5) Uani 1 1 d . . . N1 N 0.7360(17) 0.0071(6) 0.1668(9) 0.028(2) Uani 1 1 d . . . N2 N 0.740(2) 0.1399(5) 0.3869(8) 0.026(2) Uani 1 1 d . . . N3 N 0.745(2) 0.1297(5) -0.1123(8) 0.030(2) Uani 1 1 d . . . N4 N 0.7389(19) 0.2665(7) 0.1210(10) 0.034(2) Uani 1 1 d . . . N5 N 0.4267(11) 0.1366(7) 0.139(2) 0.017(3) Uani 1 1 d . . . N6 N 1.0484(11) 0.1362(7) 0.134(2) 0.020(3) Uani 1 1 d . . . N10 N 0.651(3) -0.0947(13) 0.362(2) 0.041(6) Uiso 0.70 1 d P . 1 N11 N 0.844(2) 0.0892(10) -0.3674(19) 0.012(4) Uiso 0.60 1 d P . 1 N10' N 0.714(6) -0.091(2) 0.372(4) 0.028(12) Uiso 0.30 1 d P . 2 N11' N 0.778(5) 0.0733(18) -0.366(3) 0.043(9) Uiso 0.40 1 d P . 2 C1 C 0.7096(15) -0.0418(9) 0.2569(15) 0.032(4) Uani 1 1 d . . . C2 C 0.773(3) 0.1177(7) 0.5048(10) 0.026(3) Uani 1 1 d . . . C3 C 0.773(3) 0.1116(8) -0.2360(12) 0.035(4) Uani 1 1 d . . . C4 C 0.7776(15) 0.3314(10) 0.1357(13) 0.029(3) Uani 1 1 d . . . C20 C 1.1458(16) 0.0971(11) 0.2363(16) 0.028(4) Uani 1 1 d . . . C21 C 0.3296(18) 0.0947(9) 0.2387(16) 0.024(4) Uani 1 1 d . . . C22 C 0.3348(18) 0.1812(10) 0.0357(14) 0.020(4) Uani 1 1 d . . . C23 C 1.1472(19) 0.1796(11) 0.0311(19) 0.026(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 Mn1 0.0191(8) 0.0296(11) 0.0077(7) 0.0011(7) -0.0019(12) -0.0015(11) N1 0.031(5) 0.024(7) 0.029(5) 0.001(4) 0.000(6) 0.000(6) N2 0.035(7) 0.031(6) 0.012(4) 0.001(4) 0.000(8) -0.005(7) N3 0.032(6) 0.038(7) 0.021(5) -0.001(4) -0.001(9) 0.000(8) N4 0.041(6) 0.038(8) 0.023(4) -0.012(6) 0.006(9) -0.010(7) N5 0.026(5) 0.010(7) 0.016(6) 0.006(7) -0.010(7) 0.003(5) N6 0.012(5) 0.023(7) 0.026(7) 0.003(8) -0.011(5) 0.004(5) C1 0.024(8) 0.030(10) 0.042(7) -0.028(7) 0.000(6) 0.005(6) C2 0.043(9) 0.032(9) 0.002(5) -0.003(4) 0.001(7) -0.004(9) C3 0.052(10) 0.038(9) 0.015(6) 0.003(5) 0.001(10) 0.012(10) C4 0.021(8) 0.049(11) 0.018(5) 0.002(6) 0.011(8) -0.007(6) C20 0.016(7) 0.047(12) 0.023(8) 0.023(8) 0.001(6) 0.000(6) C21 0.040(8) 0.011(10) 0.021(8) -0.009(8) 0.005(6) 0.005(6) C22 0.025(8) 0.030(12) 0.006(7) 0.012(7) 0.001(5) -0.006(6) C23 0.026(9) 0.011(11) 0.041(10) -0.014(9) 0.005(7) -0.001(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 Mn1 N3 2.173(7) . ? Mn1 N4 2.177(11) . ? Mn1 N1 2.220(10) . ? Mn1 N2 2.227(7) . ? Mn1 N6 2.272(8) . ? Mn1 N5 2.299(9) . ? N1 C1 1.161(16) . ? N2 C2 1.131(13) . ? N3 C3 1.149(13) . ? N4 C4 1.139(15) . ? N5 C21 1.333(19) . ? N5 C22 1.360(18) . ? N6 C20 1.33(2) . ? N6 C23 1.37(2) . ? N10 C4 1.35(2) 2_645 ? N10 C1 1.36(3) . ? N11 C3 1.33(2) . ? N11 C2 1.33(2) 1_554 ? N10' C1 1.31(4) . ? N10' C4 1.31(4) 2_645 ? N11' C3 1.32(3) . ? N11' C2 1.36(3) 1_554 ? C2 N11 1.33(2) 1_556 ? C2 N11' 1.36(3) 1_556 ? C4 N10 1.35(2) 2_655 ? C4 N10' 1.31(4) 2_655 ? C20 C21 1.352(14) 1_655 ? C21 C20 1.352(14) 1_455 ? C22 C23 1.380(14) 1_455 ? C23 C22 1.380(14) 1_655 ? 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 N4 90.5(3) . . ? N3 Mn1 N1 94.0(3) . . ? N4 Mn1 N1 175.5(3) . . ? N3 Mn1 N2 177.2(4) . . ? N4 Mn1 N2 92.0(3) . . ? N1 Mn1 N2 83.5(3) . . ? N3 Mn1 N6 88.7(7) . . ? N4 Mn1 N6 90.7(5) . . ? N1 Mn1 N6 90.1(4) . . ? N2 Mn1 N6 90.1(6) . . ? N3 Mn1 N5 92.3(6) . . ? N4 Mn1 N5 90.4(4) . . ? N1 Mn1 N5 88.8(4) . . ? N2 Mn1 N5 88.9(6) . . ? N6 Mn1 N5 178.5(3) . . ? C1 N1 Mn1 142.6(9) . . ? C2 N2 Mn1 155.8(12) . . ? C3 N3 Mn1 164.9(13) . . ? C4 N4 Mn1 162.6(13) . . ? C21 N5 C22 117.8(10) . . ? C21 N5 Mn1 123.6(10) . . ? C22 N5 Mn1 118.6(10) . . ? C20 N6 C23 115.3(11) . . ? C20 N6 Mn1 122.9(11) . . ? C23 N6 Mn1 121.7(11) . . ? C4 N10 C1 119.3(17) 2_645 . ? C3 N11 C2 118.7(14) . 1_554 ? C1 N10' C4 127(3) . 2_645 ? C3 N11' C2 117(2) . 1_554 ? N1 C1 N10' 167(2) . . ? N1 C1 N10 170.8(16) . . ? N10' C1 N10 20.3(19) . . ? N2 C2 N11 169(2) . 1_556 ? N2 C2 N11' 162(2) . 1_556 ? N11 C2 N11' 23.8(13) 1_556 1_556 ? N3 C3 N11' 164(2) . . ? N3 C3 N11 167(2) . . ? N11' C3 N11 24.2(14) . . ? N4 C4 N10 169.8(15) . 2_655 ? N4 C4 N10' 165(2) . 2_655 ? N10 C4 N10' 20.4(19) 2_655 2_655 ? N6 C20 C21 124.3(16) . 1_655 ? N5 C21 C20 120.7(16) . 1_455 ? N5 C22 C23 120.3(16) . 1_455 ? C22 C23 N6 121.4(18) 1_655 . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.905 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.186