# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 loop_ _publ_author_name 'Dai-Zheng Liao' 'Peng Cheng' 'Wen Dong' 'Zong-Hui Jiang' 'Ya-Qiu Sun' ; Shi-Ping Yan ; 'Li-Na Zhu' _publ_contact_author_name 'Prof Dai-Zheng Liao' _publ_contact_author_address ; Department of Chemistry Nankai University Weijin Road 94 Tianjin 300071 CHINA ; _publ_contact_author_email COORD@NANKAI.EDU.CN _publ_section_title ; Two different three-dimensional microporous framework structures in {Mn2(H2O)4 [W(CN)8]. 4H2O}n and {Mn2(H2O)4 [W(CN)8](OH)2H2O}n ; data_021209e _database_code_CSD 212604 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H13 Mn2 N8 O7 W' _chemical_formula_weight 626.99 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' O O 0.0106 0.0060 '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' W W -0.8490 6.8722 '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 7.3159(10) _cell_length_b 14.3390(17) _cell_length_c 18.052(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.067(7) _cell_angle_gamma 90.00 _cell_volume 1893.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 598 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 23.72 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 7.421 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.701860 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _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 5944 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.1013 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3246 _reflns_number_gt 2316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0456P)^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_number_reflns 3246 _refine_ls_number_parameters 235 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.103 _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 W1 W 0.24346(5) 0.66155(3) 0.83348(2) 0.00893(15) Uani 1 1 d . . . Mn1 Mn 0.2489(2) 0.80503(13) 0.55432(9) 0.0139(4) Uani 1 1 d . . . Mn2 Mn -0.2712(2) 0.43471(13) 0.70352(10) 0.0150(4) Uani 1 1 d . . . O1 O 0.5273(10) 0.8027(8) 0.6099(5) 0.044(3) Uani 1 1 d . . . O2 O 0.3025(12) 0.6566(7) 0.5177(5) 0.034(2) Uani 1 1 d . . . O3 O -0.1706(10) 0.4798(7) 0.5930(4) 0.029(2) Uani 1 1 d . . . O4 O -0.3501(11) 0.3719(7) 0.8114(5) 0.033(2) Uani 1 1 d . . . C1 C 0.0357(14) 0.5759(9) 0.7832(7) 0.020(3) Uani 1 1 d . . . N1 N -0.0695(12) 0.5243(8) 0.7590(6) 0.028(3) Uani 1 1 d . . . C2 C 0.1884(14) 0.7138(9) 0.7202(7) 0.017(3) Uani 1 1 d . . . N2 N 0.1655(13) 0.7409(8) 0.6609(6) 0.024(3) Uani 1 1 d . . . C3 C 0.4354(14) 0.5863(9) 0.7671(7) 0.018(3) Uani 1 1 d . . . N3 N 0.5260(12) 0.5445(8) 0.7259(6) 0.025(3) Uani 1 1 d . . . C4 C 0.4554(13) 0.7641(9) 0.8144(6) 0.014(3) Uani 1 1 d . . . N4 N 0.5670(13) 0.8188(7) 0.8041(6) 0.027(3) Uani 1 1 d . . . C5 C 0.4061(15) 0.6826(9) 0.9332(7) 0.018(3) Uani 1 1 d . . . N5 N 0.4926(12) 0.6938(8) 0.9863(6) 0.022(2) Uani 1 1 d U . . C6 C 0.0916(14) 0.7876(9) 0.8445(6) 0.013(3) Uani 1 1 d U . . N6 N -0.0041(12) 0.8525(8) 0.8482(6) 0.025(3) Uani 1 1 d . . . C7 C 0.0353(14) 0.6502(9) 0.9188(7) 0.019(3) Uani 1 1 d . . . N7 N -0.0764(12) 0.6482(8) 0.9623(6) 0.026(3) Uani 1 1 d . . . C8 C 0.2816(14) 0.5214(10) 0.8820(7) 0.019(3) Uani 1 1 d . . . N8 N 0.2958(14) 0.4497(8) 0.9062(6) 0.025(3) Uani 1 1 d . . . O5 O 0.2143(12) 0.4989(8) 0.5966(5) 0.042(3) Uani 1 1 d . . . O6 O 0.2857(14) 0.3641(8) 0.4784(6) 0.057(3) Uani 1 1 d . . . O7 O 0.2484(15) 0.0361(9) 0.4305(6) 0.061(3) 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 W1 0.0101(2) 0.0093(3) 0.0074(3) 0.0003(3) -0.00124(14) -0.0005(2) Mn1 0.0168(8) 0.0154(11) 0.0095(10) 0.0004(8) -0.0005(7) 0.0007(7) Mn2 0.0134(8) 0.0149(11) 0.0167(11) -0.0044(9) -0.0012(7) -0.0002(7) O1 0.024(5) 0.076(9) 0.034(6) -0.007(6) -0.017(4) -0.012(5) O2 0.050(5) 0.024(6) 0.027(6) 0.002(5) 0.004(4) 0.004(5) O3 0.031(4) 0.037(6) 0.017(5) 0.005(5) 0.001(4) -0.007(4) O4 0.038(5) 0.038(7) 0.024(6) 0.012(5) 0.004(4) -0.005(5) C1 0.015(5) 0.017(8) 0.027(8) 0.001(6) 0.005(5) 0.001(6) N1 0.021(5) 0.023(7) 0.039(7) -0.001(6) -0.008(5) -0.012(5) C2 0.015(5) 0.011(7) 0.026(8) 0.001(6) -0.006(5) 0.002(5) N2 0.032(6) 0.028(7) 0.013(7) 0.007(6) -0.005(4) -0.001(5) C3 0.018(6) 0.019(8) 0.018(7) 0.004(6) 0.004(5) -0.006(5) N3 0.021(5) 0.019(7) 0.036(7) -0.004(6) 0.004(5) 0.003(5) C4 0.013(5) 0.011(7) 0.016(7) 0.000(6) -0.003(5) -0.008(5) N4 0.028(5) 0.023(7) 0.030(7) -0.008(5) 0.007(5) -0.009(5) C5 0.023(6) 0.017(8) 0.014(7) 0.004(6) 0.001(5) -0.003(5) N5 0.023(3) 0.022(3) 0.020(3) 0.0009(19) -0.0027(19) 0.0002(19) C6 0.014(3) 0.014(3) 0.013(3) 0.0001(19) -0.0010(19) -0.0004(19) N6 0.023(5) 0.027(7) 0.025(6) -0.004(6) -0.001(4) 0.002(5) C7 0.015(5) 0.014(8) 0.028(8) 0.003(6) -0.001(5) 0.002(5) N7 0.022(5) 0.031(8) 0.025(6) -0.001(6) 0.007(5) 0.001(5) C8 0.015(5) 0.022(8) 0.020(8) -0.005(7) -0.001(5) -0.002(6) N8 0.041(6) 0.015(7) 0.019(7) 0.004(6) 0.008(5) 0.004(5) O5 0.042(5) 0.047(8) 0.036(6) 0.011(5) -0.011(5) 0.001(5) O6 0.058(6) 0.055(8) 0.058(8) 0.017(7) 0.005(6) 0.023(6) O7 0.076(8) 0.064(9) 0.044(7) 0.013(7) 0.003(6) 0.016(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 W1 C6 2.133(12) . ? W1 C1 2.143(13) . ? W1 C3 2.153(12) . ? W1 C4 2.169(11) . ? W1 C5 2.160(12) . ? W1 C7 2.192(11) . ? W1 C2 2.208(13) . ? W1 C8 2.208(14) . ? Mn1 N8 2.219(12) 2_556 ? Mn1 N7 2.219(10) 4_675 ? Mn1 N5 2.222(10) 4_575 ? Mn1 N2 2.228(11) . ? Mn1 O1 2.253(8) . ? Mn1 O2 2.265(10) . ? Mn2 N1 2.185(10) . ? Mn2 N3 2.205(10) 1_455 ? Mn2 N6 2.215(10) 2_446 ? Mn2 O4 2.231(9) . ? Mn2 O3 2.236(8) . ? Mn2 N4 2.241(10) 2_546 ? C1 N1 1.148(15) . ? C2 N2 1.148(14) . ? C3 N3 1.171(14) . ? N3 Mn2 2.205(10) 1_655 ? C4 N4 1.150(14) . ? N4 Mn2 2.241(10) 2_556 ? C5 N5 1.151(14) . ? N5 Mn1 2.222(10) 4_676 ? C6 N6 1.167(15) . ? N6 Mn2 2.215(10) 2_456 ? C7 N7 1.144(14) . ? N7 Mn1 2.219(10) 4_576 ? C8 N8 1.121(16) . ? N8 Mn1 2.219(12) 2_546 ? 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 C6 W1 C1 99.2(4) . . ? C6 W1 C3 145.4(4) . . ? C1 W1 C3 86.7(4) . . ? C6 W1 C4 79.4(4) . . ? C1 W1 C4 145.6(4) . . ? C3 W1 C4 77.0(4) . . ? C6 W1 C5 94.8(4) . . ? C1 W1 C5 143.9(5) . . ? C3 W1 C5 100.3(4) . . ? C4 W1 C5 69.7(4) . . ? C6 W1 C7 68.1(4) . . ? C1 W1 C7 76.0(4) . . ? C3 W1 C7 145.4(5) . . ? C4 W1 C7 132.0(4) . . ? C5 W1 C7 78.7(4) . . ? C6 W1 C2 73.3(4) . . ? C1 W1 C2 71.7(4) . . ? C3 W1 C2 76.3(4) . . ? C4 W1 C2 75.1(4) . . ? C5 W1 C2 144.3(4) . . ? C7 W1 C2 124.0(4) . . ? C6 W1 C8 142.8(4) . . ? C1 W1 C8 74.3(4) . . ? C3 W1 C8 71.7(4) . . ? C4 W1 C8 126.5(4) . . ? C5 W1 C8 74.5(4) . . ? C7 W1 C8 74.8(4) . . ? C2 W1 C8 134.1(5) . . ? N8 Mn1 N7 92.8(4) 2_556 4_675 ? N8 Mn1 N5 92.4(4) 2_556 4_575 ? N7 Mn1 N5 94.4(4) 4_675 4_575 ? N8 Mn1 N2 93.6(4) 2_556 . ? N7 Mn1 N2 160.5(4) 4_675 . ? N5 Mn1 N2 103.8(4) 4_575 . ? N8 Mn1 O1 90.5(4) 2_556 . ? N7 Mn1 O1 79.0(4) 4_675 . ? N5 Mn1 O1 172.9(4) 4_575 . ? N2 Mn1 O1 82.5(4) . . ? N8 Mn1 O2 177.8(4) 2_556 . ? N7 Mn1 O2 87.7(4) 4_675 . ? N5 Mn1 O2 89.7(4) 4_575 . ? N2 Mn1 O2 85.2(4) . . ? O1 Mn1 O2 87.5(4) . . ? N1 Mn2 N3 87.0(4) . 1_455 ? N1 Mn2 N6 174.6(4) . 2_446 ? N3 Mn2 N6 87.8(4) 1_455 2_446 ? N1 Mn2 O4 91.2(4) . . ? N3 Mn2 O4 86.7(4) 1_455 . ? N6 Mn2 O4 87.2(4) 2_446 . ? N1 Mn2 O3 90.5(4) . . ? N3 Mn2 O3 101.0(4) 1_455 . ? N6 Mn2 O3 91.8(3) 2_446 . ? O4 Mn2 O3 172.2(4) . . ? N1 Mn2 N4 91.1(4) . 2_546 ? N3 Mn2 N4 172.8(4) 1_455 2_546 ? N6 Mn2 N4 94.0(4) 2_446 2_546 ? O4 Mn2 N4 86.4(4) . 2_546 ? O3 Mn2 N4 85.9(4) . 2_546 ? N1 C1 W1 174.8(11) . . ? C1 N1 Mn2 174.5(11) . . ? N2 C2 W1 177.9(9) . . ? C2 N2 Mn1 155.1(9) . . ? N3 C3 W1 173.4(10) . . ? C3 N3 Mn2 150.8(10) . 1_655 ? N4 C4 W1 179.6(12) . . ? C4 N4 Mn2 172.8(10) . 2_556 ? N5 C5 W1 179.9(13) . . ? C5 N5 Mn1 155.1(9) . 4_676 ? N6 C6 W1 174.2(10) . . ? C6 N6 Mn2 147.4(9) . 2_456 ? N7 C7 W1 176.8(11) . . ? C7 N7 Mn1 159.2(11) . 4_576 ? N8 C8 W1 178.0(11) . . ? C8 N8 Mn1 165.7(10) . 2_546 ? 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 C6 W1 C1 N1 -148(12) . . . . ? C3 W1 C1 N1 66(12) . . . . ? C4 W1 C1 N1 127(12) . . . . ? C5 W1 C1 N1 -37(12) . . . . ? C7 W1 C1 N1 -84(12) . . . . ? C2 W1 C1 N1 143(12) . . . . ? C8 W1 C1 N1 -6(12) . . . . ? W1 C1 N1 Mn2 -148(8) . . . . ? N3 Mn2 N1 C1 -73(11) 1_455 . . . ? N6 Mn2 N1 C1 -87(11) 2_446 . . . ? O4 Mn2 N1 C1 -160(11) . . . . ? O3 Mn2 N1 C1 28(11) . . . . ? N4 Mn2 N1 C1 114(11) 2_546 . . . ? C6 W1 C2 N2 124(31) . . . . ? C1 W1 C2 N2 -130(31) . . . . ? C3 W1 C2 N2 -39(31) . . . . ? C4 W1 C2 N2 41(31) . . . . ? C5 W1 C2 N2 49(31) . . . . ? C7 W1 C2 N2 172(30) . . . . ? C8 W1 C2 N2 -86(31) . . . . ? W1 C2 N2 Mn1 -16(33) . . . . ? N8 Mn1 N2 C2 -87(3) 2_556 . . . ? N7 Mn1 N2 C2 22(3) 4_675 . . . ? N5 Mn1 N2 C2 179(3) 4_575 . . . ? O1 Mn1 N2 C2 3(3) . . . . ? O2 Mn1 N2 C2 91(3) . . . . ? C6 W1 C3 N3 -71(9) . . . . ? C1 W1 C3 N3 30(9) . . . . ? C4 W1 C3 N3 -119(9) . . . . ? C5 W1 C3 N3 175(9) . . . . ? C7 W1 C3 N3 90(9) . . . . ? C2 W1 C3 N3 -42(9) . . . . ? C8 W1 C3 N3 105(9) . . . . ? W1 C3 N3 Mn2 -136(8) . . . 1_655 ? C6 W1 C4 N4 -41(100) . . . . ? C1 W1 C4 N4 50(100) . . . . ? C3 W1 C4 N4 114(100) . . . . ? C5 W1 C4 N4 -140(100) . . . . ? C7 W1 C4 N4 -88(100) . . . . ? C2 W1 C4 N4 35(100) . . . . ? C8 W1 C4 N4 169(100) . . . . ? W1 C4 N4 Mn2 87(100) . . . 2_556 ? C6 W1 C5 N5 76(100) . . . . ? C1 W1 C5 N5 -36(100) . . . . ? C3 W1 C5 N5 -135(100) . . . . ? C4 W1 C5 N5 153(100) . . . . ? C7 W1 C5 N5 10(100) . . . . ? C2 W1 C5 N5 144(100) . . . . ? C8 W1 C5 N5 -67(100) . . . . ? W1 C5 N5 Mn1 148(100) . . . 4_676 ? C1 W1 C6 N6 3(10) . . . . ? C3 W1 C6 N6 100(10) . . . . ? C4 W1 C6 N6 148(10) . . . . ? C5 W1 C6 N6 -144(10) . . . . ? C7 W1 C6 N6 -68(10) . . . . ? C2 W1 C6 N6 71(10) . . . . ? C8 W1 C6 N6 -73(10) . . . . ? W1 C6 N6 Mn2 -39(11) . . . 2_456 ? C6 W1 C7 N7 8(20) . . . . ? C1 W1 C7 N7 -98(20) . . . . ? C3 W1 C7 N7 -160(20) . . . . ? C4 W1 C7 N7 59(20) . . . . ? C5 W1 C7 N7 108(20) . . . . ? C2 W1 C7 N7 -42(20) . . . . ? C8 W1 C7 N7 -175(20) . . . . ? W1 C7 N7 Mn1 -50(22) . . . 4_576 ? C6 W1 C8 N8 63(34) . . . . ? C1 W1 C8 N8 -21(33) . . . . ? C3 W1 C8 N8 -113(33) . . . . ? C4 W1 C8 N8 -171(33) . . . . ? C5 W1 C8 N8 140(33) . . . . ? C7 W1 C8 N8 58(33) . . . . ? C2 W1 C8 N8 -65(33) . . . . ? W1 C8 N8 Mn1 -2(37) . . . 2_546 ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.481 _refine_diff_density_min -1.826 _refine_diff_density_rms 0.261 data_030513c _database_code_CSD 212605 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 Mn2 N8 O8 W' _chemical_formula_weight 646.02 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' O O 0.0106 0.0060 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 11.915(4) _cell_length_b 11.915(4) _cell_length_c 13.252(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1881.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 834 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 26.45 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 7.476 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.583960 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _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 5434 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 26.45 _reflns_number_total 1025 _reflns_number_gt 863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0151P)^2^+11.2882P] 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_number_reflns 1025 _refine_ls_number_parameters 67 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _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 W1 W 1.0000 0.0000 0.24849(3) 0.00936(10) Uani 1 4 d S . . C1 C 0.9233(4) 0.1314(4) 0.3371(3) 0.0189(9) Uani 1 1 d . . . N1 N 0.8765(4) 0.1985(4) 0.3815(3) 0.0331(11) Uani 1 1 d . . . C2 C 0.8560(4) 0.0495(4) 0.1600(3) 0.0190(9) Uani 1 1 d . . . N2 N 0.7812(3) 0.0817(4) 0.1135(3) 0.0280(10) Uani 1 1 d . . . Mn1 Mn 0.80328(8) 0.30638(8) 0.5000 0.0162(2) Uani 1 2 d S . . O1 O 0.9617(5) 0.3933(6) 0.5000 0.084(3) Uani 1 2 d S . . H1A H 1.0226 0.3562 0.5000 0.100 Uiso 1 2 d SR . . H1B H 0.9634 0.4646 0.5000 0.100 Uiso 1 2 d SR . . O2 O 0.6456(5) 0.2094(5) 0.5000 0.0461(15) Uani 1 2 d S . . H2A H 0.6380 0.1537 0.4605 0.055 Uiso 0.50 1 d PR . . H2B H 0.5924 0.2277 0.5395 0.055 Uiso 0.50 1 d PR . . O3 O 0.0965(5) 0.3823(4) 0.3051(4) 0.0763(16) Uani 1 1 d . . . H3A H 0.1037 0.4438 0.2732 0.114 Uiso 1 1 d R . . H3B H 0.1272 0.3302 0.2710 0.114 Uiso 1 1 d 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 W1 0.00940(12) 0.00940(12) 0.00929(15) 0.000 0.000 0.000 C1 0.020(2) 0.023(2) 0.014(2) -0.0009(18) 0.0048(18) 0.0005(19) N1 0.040(3) 0.029(2) 0.029(2) -0.006(2) 0.008(2) 0.010(2) C2 0.022(2) 0.019(2) 0.016(2) 0.0019(18) 0.0003(19) 0.0018(18) N2 0.023(2) 0.037(3) 0.024(2) 0.0041(19) -0.0035(18) 0.0111(18) Mn1 0.0176(5) 0.0167(5) 0.0144(4) 0.000 0.000 0.0065(4) O1 0.039(4) 0.044(4) 0.168(8) 0.000 0.000 -0.013(3) O2 0.028(3) 0.038(3) 0.072(4) 0.000 0.000 -0.003(3) O3 0.106(5) 0.060(3) 0.064(3) -0.008(3) -0.009(3) -0.004(3) _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 W1 C2 2.160(4) 3_645 ? W1 C2 2.160(4) . ? W1 C2 2.160(4) 4_665 ? W1 C2 2.160(4) 2_755 ? W1 C1 2.160(5) 4_665 ? W1 C1 2.160(5) 3_645 ? W1 C1 2.160(5) . ? W1 C1 2.160(5) 2_755 ? C1 N1 1.138(6) . ? N1 Mn1 2.209(4) . ? C2 N2 1.150(6) . ? N2 Mn1 2.248(4) 13_655 ? Mn1 O1 2.153(6) . ? Mn1 O2 2.206(6) . ? Mn1 N1 2.209(4) 10_556 ? Mn1 N2 2.248(4) 6_655 ? Mn1 N2 2.248(4) 13_655 ? O1 H1A 0.8500 . ? O1 H1B 0.8500 . ? O2 H2A 0.8499 . ? O2 H2B 0.8500 . ? O3 H3A 0.8503 . ? O3 H3B 0.8501 . ? 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 C2 W1 C2 72.84(11) 3_645 . ? C2 W1 C2 114.2(2) 3_645 4_665 ? C2 W1 C2 72.84(11) . 4_665 ? C2 W1 C2 72.84(11) 3_645 2_755 ? C2 W1 C2 114.2(2) . 2_755 ? C2 W1 C2 72.84(11) 4_665 2_755 ? C2 W1 C1 146.00(17) 3_645 4_665 ? C2 W1 C1 139.07(17) . 4_665 ? C2 W1 C1 76.20(17) 4_665 4_665 ? C2 W1 C1 80.51(17) 2_755 4_665 ? C2 W1 C1 76.20(17) 3_645 3_645 ? C2 W1 C1 80.51(17) . 3_645 ? C2 W1 C1 146.00(17) 4_665 3_645 ? C2 W1 C1 139.07(17) 2_755 3_645 ? C1 W1 C1 114.1(2) 4_665 3_645 ? C2 W1 C1 139.07(17) 3_645 . ? C2 W1 C1 76.20(17) . . ? C2 W1 C1 80.51(17) 4_665 . ? C2 W1 C1 146.00(17) 2_755 . ? C1 W1 C1 72.81(12) 4_665 . ? C1 W1 C1 72.81(12) 3_645 . ? C2 W1 C1 80.51(17) 3_645 2_755 ? C2 W1 C1 146.00(17) . 2_755 ? C2 W1 C1 139.07(17) 4_665 2_755 ? C2 W1 C1 76.20(17) 2_755 2_755 ? C1 W1 C1 72.81(12) 4_665 2_755 ? C1 W1 C1 72.81(12) 3_645 2_755 ? C1 W1 C1 114.1(2) . 2_755 ? N1 C1 W1 175.6(4) . . ? C1 N1 Mn1 165.8(4) . . ? N2 C2 W1 176.3(4) . . ? C2 N2 Mn1 154.7(4) . 13_655 ? O1 Mn1 O2 177.2(3) . . ? O1 Mn1 N1 86.22(19) . . ? O2 Mn1 N1 91.80(16) . . ? O1 Mn1 N1 86.22(19) . 10_556 ? O2 Mn1 N1 91.80(16) . 10_556 ? N1 Mn1 N1 90.6(2) . 10_556 ? O1 Mn1 N2 96.15(19) . 6_655 ? O2 Mn1 N2 85.94(16) . 6_655 ? N1 Mn1 N2 176.08(17) . 6_655 ? N1 Mn1 N2 92.65(15) 10_556 6_655 ? O1 Mn1 N2 96.15(19) . 13_655 ? O2 Mn1 N2 85.94(16) . 13_655 ? N1 Mn1 N2 92.65(15) . 13_655 ? N1 Mn1 N2 176.08(17) 10_556 13_655 ? N2 Mn1 N2 84.0(2) 6_655 13_655 ? Mn1 O1 H1A 119.9 . . ? Mn1 O1 H1B 120.1 . . ? H1A O1 H1B 120.0 . . ? Mn1 O2 H2A 120.0 . . ? Mn1 O2 H2B 120.0 . . ? H2A O2 H2B 120.0 . . ? H3A O3 H3B 108.7 . . ? 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 C2 W1 C1 N1 -9(6) 3_645 . . . ? C2 W1 C1 N1 32(6) . . . . ? C2 W1 C1 N1 107(6) 4_665 . . . ? C2 W1 C1 N1 145(5) 2_755 . . . ? C1 W1 C1 N1 -175(5) 4_665 . . . ? C1 W1 C1 N1 -52(6) 3_645 . . . ? C1 W1 C1 N1 -113(6) 2_755 . . . ? W1 C1 N1 Mn1 118(5) . . . . ? C2 W1 C2 N2 -158(6) 3_645 . . . ? C2 W1 C2 N2 -35(6) 4_665 . . . ? C2 W1 C2 N2 -97(6) 2_755 . . . ? C1 W1 C2 N2 7(6) 4_665 . . . ? C1 W1 C2 N2 123(6) 3_645 . . . ? C1 W1 C2 N2 49(6) . . . . ? C1 W1 C2 N2 162(6) 2_755 . . . ? W1 C2 N2 Mn1 40(7) . . . 13_655 ? C1 N1 Mn1 O1 83.4(18) . . . . ? C1 N1 Mn1 O2 -94.6(18) . . . . ? C1 N1 Mn1 N1 -2.8(19) . . . 10_556 ? C1 N1 Mn1 N2 -149(2) . . . 6_655 ? C1 N1 Mn1 N2 179.4(18) . . . 13_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.753 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.122