# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Banerjee, Pradyot' 'Gao, Song' 'Panja, Anangamohan' 'Shaikh, Nizamuddin' 'Vojti_ek, Pavel' _publ_contact_author_name 'Prof Pradyot Banerjee' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Kolkata 700 032 INDIA ; _publ_contact_author_email 'ICPB@MAHENDRA.IACS.RES.IN' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Synthesis, crystal structure and magnetic properties of 1D polymeric [MnIII(salen)N3] and [MnIII(salen)Ag(CN)2] complexes ; data_ns3end _database_code_CSD 188032 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 Mn N5 O2' _chemical_formula_weight 363.26 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 10.9390(3) _cell_length_b 12.9470(2) _cell_length_c 11.1140(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1574.04(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20584 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3601 _reflns_number_gt 3193 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0403P)^2^+0.1134P] 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 0.0102(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(19) _refine_ls_number_reflns 3601 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.24675(3) 0.176910(19) 0.0560 0.02803(10) Uani 1 1 d . . . O1 O 0.17102(13) 0.07537(11) 0.15048(14) 0.0322(3) Uani 1 1 d . . . O2 O 0.12634(15) 0.27792(11) 0.08698(15) 0.0413(4) Uani 1 1 d . . . N1 N 0.38794(15) 0.08478(13) 0.02164(15) 0.0304(4) Uani 1 1 d . . . N2 N 0.33847(17) 0.27187(14) -0.05024(16) 0.0331(4) Uani 1 1 d . . . C1 C 0.2061(2) -0.02063(15) 0.17453(19) 0.0296(4) Uani 1 1 d . . . C2 C 0.1328(2) -0.08046(17) 0.2505(2) 0.0361(5) Uani 1 1 d . . . C3 C 0.1632(2) -0.18071(18) 0.2797(2) 0.0456(6) Uani 1 1 d . . . C4 C 0.2684(2) -0.2249(2) 0.2323(3) 0.0487(6) Uani 1 1 d . . . C5 C 0.3429(2) -0.16872(17) 0.1566(2) 0.0418(5) Uani 1 1 d . . . C6 C 0.31317(18) -0.06593(16) 0.12698(19) 0.0315(4) Uani 1 1 d . . . C7 C 0.39956(17) -0.01048(14) 0.0539(2) 0.0324(4) Uani 1 1 d . . . C8 C 0.4900(2) 0.13712(19) -0.0403(2) 0.0357(5) Uani 1 1 d . . . C9 C 0.4346(2) 0.2200(2) -0.12043(19) 0.0386(5) Uani 1 1 d . . . C10 C 0.3171(2) 0.36872(19) -0.0635(2) 0.0438(6) Uani 1 1 d . . . C11 C 0.2238(2) 0.42527(19) -0.0035(3) 0.0460(6) Uani 1 1 d . . . C12 C 0.2242(3) 0.5343(2) -0.0180(4) 0.0664(9) Uani 1 1 d . . . C13 C 0.1386(4) 0.5945(2) 0.0385(4) 0.0769(11) Uani 1 1 d . . . C14 C 0.0508(4) 0.5492(2) 0.1101(3) 0.0664(9) Uani 1 1 d . . . C15 C 0.0451(3) 0.4423(2) 0.1247(3) 0.0546(7) Uani 1 1 d . . . C16 C 0.1336(2) 0.37919(16) 0.0691(2) 0.0410(5) Uani 1 1 d . . . H2 H 0.064(2) -0.0523(16) 0.278(2) 0.031(6) Uiso 1 1 d . . . H3 H 0.103(3) -0.226(2) 0.342(3) 0.059(8) Uiso 1 1 d . . . H4 H 0.289(3) -0.289(3) 0.253(3) 0.080(11) Uiso 1 1 d . . . H5 H 0.416(3) -0.2004(19) 0.118(2) 0.042(7) Uiso 1 1 d . . . H7 H 0.474(2) -0.0533(17) 0.029(2) 0.041(6) Uiso 1 1 d . . . H8A H 0.548(3) 0.1666(19) 0.018(3) 0.052(8) Uiso 1 1 d . . . H8B H 0.539(3) 0.090(2) -0.084(3) 0.047(7) Uiso 1 1 d . . . H9A H 0.387(2) 0.1877(18) -0.199(3) 0.039(6) Uiso 1 1 d . . . H9B H 0.499(3) 0.265(3) -0.147(3) 0.060(8) Uiso 1 1 d . . . H10 H 0.372(3) 0.415(2) -0.120(3) 0.060(8) Uiso 1 1 d . . . H12 H 0.295(3) 0.570(2) -0.076(3) 0.063(9) Uiso 1 1 d . . . H13 H 0.152(5) 0.665(4) 0.036(5) 0.14(2) Uiso 1 1 d . . . H14 H -0.012(3) 0.583(3) 0.148(3) 0.069(9) Uiso 1 1 d . . . H15 H -0.022(2) 0.412(2) 0.171(2) 0.041(7) Uiso 1 1 d . . . N11 N 0.14218(18) 0.12573(17) -0.11115(18) 0.0424(5) Uani 1 1 d . . . N12 N 0.14125(14) 0.18096(14) -0.1955(2) 0.0330(3) Uani 1 1 d . . . N13 N 0.14071(19) 0.23643(16) -0.27962(19) 0.0416(5) 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 Mn 0.02815(15) 0.02991(15) 0.02603(14) 0.00230(15) 0.00278(11) 0.00059(11) O1 0.0325(7) 0.0319(7) 0.0323(7) 0.0037(6) 0.0061(6) 0.0019(6) O2 0.0408(8) 0.0352(8) 0.0480(10) 0.0064(7) 0.0088(7) 0.0080(7) N1 0.0262(8) 0.0359(10) 0.0291(9) -0.0011(6) 0.0018(6) -0.0028(7) N2 0.0335(9) 0.0400(10) 0.0258(8) 0.0036(7) -0.0027(7) -0.0052(8) C1 0.0295(10) 0.0324(10) 0.0270(9) 0.0004(8) -0.0060(8) -0.0024(8) C2 0.0347(11) 0.0382(12) 0.0355(11) 0.0038(9) 0.0032(9) -0.0038(10) C3 0.0441(13) 0.0424(12) 0.0502(16) 0.0118(11) -0.0028(10) -0.0085(10) C4 0.0493(15) 0.0336(13) 0.0631(17) 0.0125(12) -0.0070(12) -0.0014(11) C5 0.0397(13) 0.0365(12) 0.0492(13) 0.0029(10) -0.0033(10) 0.0049(10) C6 0.0293(10) 0.0318(10) 0.0334(11) 0.0003(8) -0.0038(8) -0.0007(8) C7 0.0283(9) 0.0369(10) 0.0319(8) -0.0039(11) 0.0011(9) 0.0037(7) C8 0.0289(11) 0.0431(12) 0.0352(10) 0.0009(10) 0.0052(9) -0.0036(10) C9 0.0363(12) 0.0501(14) 0.0295(11) 0.0046(10) 0.0052(9) -0.0075(11) C10 0.0438(13) 0.0417(14) 0.0460(13) 0.0149(11) -0.0050(10) -0.0084(11) C11 0.0506(14) 0.0319(12) 0.0555(15) 0.0079(11) -0.0102(12) 0.0016(11) C12 0.0669(19) 0.0338(14) 0.099(3) 0.0149(15) -0.0188(18) 0.0016(13) C13 0.088(2) 0.0355(14) 0.107(3) 0.0000(18) -0.029(2) 0.0122(15) C14 0.077(2) 0.0494(17) 0.0733(19) -0.0134(15) -0.0259(17) 0.0317(17) C15 0.0609(17) 0.0508(16) 0.0520(16) -0.0026(12) -0.0096(14) 0.0228(13) C16 0.0454(12) 0.0363(10) 0.0412(13) 0.0038(10) -0.0103(11) 0.0095(9) N11 0.0412(11) 0.0542(12) 0.0317(10) 0.0008(9) -0.0053(8) -0.0096(10) N12 0.0280(8) 0.0447(9) 0.0264(8) -0.0062(8) 0.0002(10) 0.0000(7) N13 0.0462(11) 0.0483(12) 0.0302(9) -0.0004(8) -0.0010(8) 0.0077(9) _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 O1 1.8755(14) . ? Mn O2 1.8878(15) . ? Mn N2 1.9780(18) . ? Mn N1 1.9884(17) . ? Mn N11 2.280(2) . ? Mn N13 2.334(2) 3 ? O1 C1 1.328(2) . ? O2 C16 1.328(3) . ? N1 C7 1.291(3) . ? N1 C8 1.476(3) . ? N2 C10 1.284(3) . ? N2 C9 1.472(3) . ? C1 C2 1.399(3) . ? C1 C6 1.413(3) . ? C2 C3 1.379(3) . ? C2 H2 0.89(2) . ? C3 C4 1.389(4) . ? C3 H3 1.12(3) . ? C4 C5 1.378(4) . ? C4 H4 0.89(3) . ? C5 C6 1.409(3) . ? C5 H5 0.99(3) . ? C6 C7 1.438(3) . ? C7 H7 1.03(3) . ? C8 C9 1.520(3) . ? C8 H8A 0.98(3) . ? C8 H8B 0.95(3) . ? C9 H9A 1.10(3) . ? C9 H9B 0.96(3) . ? C10 C11 1.423(4) . ? C10 H10 1.06(3) . ? C11 C16 1.407(4) . ? C11 C12 1.421(4) . ? C12 C13 1.371(5) . ? C12 H12 1.11(3) . ? C13 C14 1.378(6) . ? C13 H13 0.93(5) . ? C14 C15 1.395(4) . ? C14 H14 0.92(4) . ? C15 C16 1.409(4) . ? C15 H15 0.98(3) . ? N11 N12 1.179(3) . ? N12 N13 1.179(3) . ? N13 Mn 2.334(2) 3_554 ? 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 O1 Mn O2 94.32(6) . . ? O1 Mn N2 173.73(7) . . ? O2 Mn N2 91.85(7) . . ? O1 Mn N1 91.73(6) . . ? O2 Mn N1 172.99(7) . . ? N2 Mn N1 82.20(7) . . ? O1 Mn N11 91.77(7) . . ? O2 Mn N11 89.99(8) . . ? N2 Mn N11 87.06(7) . . ? N1 Mn N11 93.38(8) . . ? O1 Mn N13 91.50(7) . 3 ? O2 Mn N13 89.80(7) . 3 ? N2 Mn N13 89.68(7) . 3 ? N1 Mn N13 86.48(7) . 3 ? N11 Mn N13 176.73(8) . 3 ? C1 O1 Mn 129.89(13) . . ? C16 O2 Mn 127.95(14) . . ? C7 N1 C8 119.60(18) . . ? C7 N1 Mn 126.60(14) . . ? C8 N1 Mn 113.67(14) . . ? C10 N2 C9 120.96(19) . . ? C10 N2 Mn 125.70(17) . . ? C9 N2 Mn 113.29(14) . . ? O1 C1 C2 118.3(2) . . ? O1 C1 C6 123.56(18) . . ? C2 C1 C6 118.12(19) . . ? C3 C2 C1 121.7(2) . . ? C3 C2 H2 120.5(14) . . ? C1 C2 H2 117.8(14) . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3 119.8(16) . . ? C4 C3 H3 120.3(16) . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4 120(2) . . ? C3 C4 H4 120(2) . . ? C4 C5 C6 120.3(2) . . ? C4 C5 H5 121.4(15) . . ? C6 C5 H5 118.2(15) . . ? C5 C6 C1 119.7(2) . . ? C5 C6 C7 116.9(2) . . ? C1 C6 C7 123.30(18) . . ? N1 C7 C6 124.71(18) . . ? N1 C7 H7 121.2(13) . . ? C6 C7 H7 114.0(13) . . ? N1 C8 C9 107.24(18) . . ? N1 C8 H8A 110.7(17) . . ? C9 C8 H8A 111.7(15) . . ? N1 C8 H8B 111.5(16) . . ? C9 C8 H8B 112.5(17) . . ? H8A C8 H8B 103(2) . . ? N2 C9 C8 107.22(16) . . ? N2 C9 H9A 104.7(14) . . ? C8 C9 H9A 112.7(13) . . ? N2 C9 H9B 114.0(18) . . ? C8 C9 H9B 108.4(18) . . ? H9A C9 H9B 110(2) . . ? N2 C10 C11 125.4(2) . . ? N2 C10 H10 121.2(17) . . ? C11 C10 H10 113.4(16) . . ? C16 C11 C10 123.7(2) . . ? C16 C11 C12 119.3(3) . . ? C10 C11 C12 117.1(3) . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 120.7(16) . . ? C11 C12 H12 118.7(16) . . ? C12 C13 C14 120.0(3) . . ? C12 C13 H13 116(4) . . ? C14 C13 H13 123(4) . . ? C13 C14 C15 121.4(3) . . ? C13 C14 H14 126(2) . . ? C15 C14 H14 113(2) . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 119.6(16) . . ? C16 C15 H15 120.8(16) . . ? O2 C16 C11 123.1(2) . . ? O2 C16 C15 117.8(2) . . ? C11 C16 C15 119.1(2) . . ? N12 N11 Mn 118.41(16) . . ? N13 N12 N11 179.7(3) . . ? N12 N13 Mn 114.65(15) . 3_554 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.198 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.042 data_ns6end _database_code_CSD 188033 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H56 Ag4 Mn4 N16 O8' _chemical_formula_weight 1924.57 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' 'Ag' 'Ag' -0.8971 1.1015 '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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 8.148(5) _cell_length_b 6.509(5) _cell_length_c 33.158(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.346(5) _cell_angle_gamma 90.00 _cell_volume 1747.8(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.863 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2802 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2802 _reflns_number_gt 2292 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0336P)^2^+2.1469P] 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 0.0007(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2802 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.21823(7) 0.49196(7) 0.125904(19) 0.0336(2) Uani 1 1 d . . . O1 O 0.3258(3) 0.6556(4) 0.16774(9) 0.0400(7) Uani 1 1 d . . . O2 O 0.2473(4) 0.6829(4) 0.08499(9) 0.0452(7) Uani 1 1 d . . . N1 N 0.1666(4) 0.2780(4) 0.16525(11) 0.0357(8) Uani 1 1 d . . . N2 N 0.1081(4) 0.2947(4) 0.08577(12) 0.0376(8) Uani 1 1 d . . . C1 C 0.2982(5) 0.6556(5) 0.20603(14) 0.0380(10) Uani 1 1 d . . . C2 C 0.3551(5) 0.8232(6) 0.23095(16) 0.0463(11) Uani 1 1 d . . . C3 C 0.3277(6) 0.8336(8) 0.27059(17) 0.0536(12) Uani 1 1 d . . . C4 C 0.2455(6) 0.6782(8) 0.28846(18) 0.0586(13) Uani 1 1 d . . . C5 C 0.1940(6) 0.5097(7) 0.26561(16) 0.0502(12) Uani 1 1 d . . . C6 C 0.2186(5) 0.4929(6) 0.22456(13) 0.0383(9) Uani 1 1 d . . . C7 C 0.1653(5) 0.3083(6) 0.20312(15) 0.0390(10) Uani 1 1 d . . . C8 C 0.1133(6) 0.0826(6) 0.14559(16) 0.0427(11) Uani 1 1 d . . . C9 C 0.0185(6) 0.1314(7) 0.10492(17) 0.0480(12) Uani 1 1 d . . . C10 C 0.1208(5) 0.2980(6) 0.04783(15) 0.0415(10) Uani 1 1 d . . . C11 C 0.2034(5) 0.4560(6) 0.02718(13) 0.0401(10) Uani 1 1 d . . . C12 C 0.2239(6) 0.4275(8) -0.01396(16) 0.0536(12) Uani 1 1 d . . . C13 C 0.2964(6) 0.5743(9) -0.03570(19) 0.0616(14) Uani 1 1 d . . . C14 C 0.3450(6) 0.7569(9) -0.01702(17) 0.0608(14) Uani 1 1 d . . . C15 C 0.3254(6) 0.7926(7) 0.02300(16) 0.0511(12) Uani 1 1 d . . . C16 C 0.2586(5) 0.6415(6) 0.04655(14) 0.0393(10) Uani 1 1 d . . . N99 N 0.4490(4) 0.3056(6) 0.11680(12) 0.0508(10) Uani 1 1 d . . . C99 C 0.5044(5) 0.1461(7) 0.11810(15) 0.0483(11) Uani 1 1 d . . . Ag Ag 0.62297(5) -0.13411(5) 0.126100(13) 0.0633(2) Uani 1 1 d . . . C98 C -0.1740(6) 0.6729(6) 0.13310(16) 0.0509(12) Uani 1 1 d . . . N98 N -0.0455(4) 0.6069(5) 0.13435(13) 0.0496(10) Uani 1 1 d . . . H91 H -0.087(6) 0.181(6) 0.1077(13) 0.044(12) Uiso 1 1 d . . . H81 H 0.045(5) 0.015(6) 0.1609(13) 0.038(11) Uiso 1 1 d . . . H10 H 0.061(5) 0.189(6) 0.0302(14) 0.043(11) Uiso 1 1 d . . . H7 H 0.136(5) 0.201(7) 0.2199(13) 0.043(11) Uiso 1 1 d . . . H4 H 0.227(5) 0.691(7) 0.3154(16) 0.051(13) Uiso 1 1 d . . . H82 H 0.212(5) -0.003(6) 0.1399(14) 0.052(12) Uiso 1 1 d . . . H2 H 0.411(4) 0.919(6) 0.2188(11) 0.025(9) Uiso 1 1 d . . . H14 H 0.396(7) 0.846(8) -0.0331(17) 0.076(17) Uiso 1 1 d . . . H3 H 0.365(5) 0.948(7) 0.2843(14) 0.047(12) Uiso 1 1 d . . . H12 H 0.191(6) 0.296(8) -0.0243(15) 0.062(14) Uiso 1 1 d . . . H15 H 0.357(5) 0.914(7) 0.0365(14) 0.043(12) Uiso 1 1 d . . . H5 H 0.149(5) 0.406(7) 0.2776(14) 0.048(13) Uiso 1 1 d . . . H13 H 0.311(6) 0.532(7) -0.0603(17) 0.056(15) Uiso 1 1 d . . . H92 H 0.007(5) 0.015(7) 0.0871(14) 0.048(12) Uiso 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 Mn 0.0399(4) 0.0215(3) 0.0399(4) 0.0013(2) 0.0067(3) 0.0012(2) O1 0.0489(16) 0.0314(14) 0.040(2) -0.0017(12) 0.0054(14) -0.0050(11) O2 0.0683(19) 0.0275(13) 0.041(2) 0.0018(12) 0.0097(15) -0.0023(12) N1 0.0380(18) 0.0233(15) 0.047(3) 0.0025(14) 0.0091(17) 0.0007(12) N2 0.0370(18) 0.0286(16) 0.048(3) -0.0018(15) 0.0072(17) 0.0015(13) C1 0.034(2) 0.034(2) 0.045(3) -0.0010(18) 0.001(2) 0.0075(15) C2 0.044(2) 0.040(2) 0.054(4) -0.004(2) 0.004(2) -0.0051(18) C3 0.050(3) 0.055(3) 0.054(4) -0.010(2) -0.003(3) -0.002(2) C4 0.053(3) 0.079(4) 0.045(4) -0.008(3) 0.008(3) -0.001(2) C5 0.042(2) 0.058(3) 0.050(3) 0.006(2) 0.008(2) 0.000(2) C6 0.035(2) 0.041(2) 0.039(3) 0.0023(18) 0.0043(19) 0.0032(16) C7 0.036(2) 0.031(2) 0.051(3) 0.011(2) 0.010(2) 0.0039(16) C8 0.049(3) 0.0239(19) 0.057(4) -0.0007(19) 0.014(2) -0.0024(17) C9 0.053(3) 0.033(2) 0.059(4) -0.002(2) 0.009(3) -0.0077(19) C10 0.040(2) 0.037(2) 0.047(3) -0.005(2) 0.003(2) 0.0015(17) C11 0.036(2) 0.045(2) 0.039(3) -0.0007(19) 0.003(2) 0.0050(17) C12 0.046(3) 0.058(3) 0.056(4) -0.006(2) 0.003(2) 0.000(2) C13 0.052(3) 0.087(4) 0.047(4) -0.004(3) 0.011(3) -0.002(3) C14 0.054(3) 0.075(4) 0.055(4) 0.014(3) 0.013(3) -0.011(2) C15 0.055(3) 0.049(3) 0.049(4) 0.007(2) 0.007(2) -0.009(2) C16 0.037(2) 0.039(2) 0.042(3) 0.0052(19) 0.003(2) 0.0063(16) N99 0.042(2) 0.047(2) 0.065(3) -0.0011(18) 0.0116(19) 0.0113(17) C99 0.035(2) 0.059(3) 0.051(3) -0.003(2) 0.008(2) 0.006(2) Ag 0.0542(3) 0.0552(3) 0.0793(4) -0.00682(19) 0.0019(2) 0.02362(16) C98 0.049(3) 0.038(2) 0.065(4) -0.006(2) 0.004(2) 0.0037(19) N98 0.041(2) 0.0382(19) 0.070(3) -0.0043(17) 0.0046(19) 0.0097(15) _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 O2 1.874(3) . ? Mn O1 1.886(3) . ? Mn N1 1.985(3) . ? Mn N2 1.990(4) . ? Mn N99 2.285(4) . ? Mn N98 2.322(4) . ? O1 C1 1.314(5) . ? O2 C16 1.316(5) . ? N1 C7 1.272(5) . ? N1 C8 1.473(5) . ? N2 C10 1.274(5) . ? N2 C9 1.472(5) . ? C1 C2 1.415(6) . ? C1 C6 1.417(5) . ? C2 C3 1.359(7) . ? C2 H2 0.89(4) . ? C3 C4 1.382(7) . ? C3 H3 0.91(5) . ? C4 C5 1.372(7) . ? C4 H4 0.93(5) . ? C5 C6 1.402(6) . ? C5 H5 0.88(4) . ? C6 C7 1.439(6) . ? C7 H7 0.94(4) . ? C8 C9 1.512(7) . ? C8 H81 0.91(4) . ? C8 H82 1.02(4) . ? C9 H91 0.93(4) . ? C9 H92 0.96(5) . ? C10 C11 1.443(6) . ? C10 H10 1.01(4) . ? C11 C12 1.405(7) . ? C11 C16 1.417(6) . ? C12 C13 1.369(7) . ? C12 H12 0.95(5) . ? C13 C14 1.378(8) . ? C13 H13 0.88(5) . ? C14 C15 1.374(7) . ? C14 H14 0.92(6) . ? C15 C16 1.403(6) . ? C15 H15 0.93(4) . ? N99 C99 1.131(5) . ? C99 Ag 2.067(5) . ? Ag C98 2.069(5) 1_645 ? C98 N98 1.128(5) . ? C98 Ag 2.069(5) 1_465 ? 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 O2 Mn O1 94.14(13) . . ? O2 Mn N1 173.74(14) . . ? O1 Mn N1 91.59(14) . . ? O2 Mn N2 91.58(14) . . ? O1 Mn N2 174.01(13) . . ? N1 Mn N2 82.77(15) . . ? O2 Mn N99 94.84(14) . . ? O1 Mn N99 94.28(14) . . ? N1 Mn N99 87.23(13) . . ? N2 Mn N99 83.46(14) . . ? O2 Mn N98 93.82(13) . . ? O1 Mn N98 95.19(13) . . ? N1 Mn N98 83.14(13) . . ? N2 Mn N98 86.19(13) . . ? N99 Mn N98 166.67(13) . . ? C1 O1 Mn 126.6(2) . . ? C16 O2 Mn 126.4(2) . . ? C7 N1 C8 122.4(3) . . ? C7 N1 Mn 124.5(3) . . ? C8 N1 Mn 112.9(3) . . ? C10 N2 C9 122.4(4) . . ? C10 N2 Mn 124.7(3) . . ? C9 N2 Mn 112.7(3) . . ? O1 C1 C2 119.0(4) . . ? O1 C1 C6 123.7(4) . . ? C2 C1 C6 117.3(4) . . ? C3 C2 C1 121.7(4) . . ? C3 C2 H2 123(2) . . ? C1 C2 H2 115(2) . . ? C2 C3 C4 121.2(5) . . ? C2 C3 H3 116(3) . . ? C4 C3 H3 123(3) . . ? C5 C4 C3 118.8(5) . . ? C5 C4 H4 122(3) . . ? C3 C4 H4 119(3) . . ? C4 C5 C6 122.0(5) . . ? C4 C5 H5 118(3) . . ? C6 C5 H5 119(3) . . ? C5 C6 C1 118.9(4) . . ? C5 C6 C7 118.5(4) . . ? C1 C6 C7 122.6(4) . . ? N1 C7 C6 125.6(4) . . ? N1 C7 H7 120(3) . . ? C6 C7 H7 114(3) . . ? N1 C8 C9 108.0(3) . . ? N1 C8 H81 110(2) . . ? C9 C8 H81 109(3) . . ? N1 C8 H82 111(2) . . ? C9 C8 H82 107(3) . . ? H81 C8 H82 113(3) . . ? N2 C9 C8 107.9(4) . . ? N2 C9 H91 107(3) . . ? C8 C9 H91 112(3) . . ? N2 C9 H92 109(3) . . ? C8 C9 H92 113(3) . . ? H91 C9 H92 108(4) . . ? N2 C10 C11 125.0(4) . . ? N2 C10 H10 118(2) . . ? C11 C10 H10 117(2) . . ? C12 C11 C16 119.1(4) . . ? C12 C11 C10 118.6(4) . . ? C16 C11 C10 122.2(4) . . ? C13 C12 C11 121.6(5) . . ? C13 C12 H12 124(3) . . ? C11 C12 H12 114(3) . . ? C12 C13 C14 119.0(5) . . ? C12 C13 H13 112(3) . . ? C14 C13 H13 129(3) . . ? C15 C14 C13 121.4(5) . . ? C15 C14 H14 124(3) . . ? C13 C14 H14 114(3) . . ? C14 C15 C16 120.9(5) . . ? C14 C15 H15 123(3) . . ? C16 C15 H15 116(3) . . ? O2 C16 C15 117.9(4) . . ? O2 C16 C11 124.1(4) . . ? C15 C16 C11 117.9(4) . . ? C99 N99 Mn 144.4(3) . . ? N99 C99 Ag 173.5(4) . . ? C99 Ag C98 154.99(17) . 1_645 ? N98 C98 Ag 164.2(4) . 1_465 ? C98 N98 Mn 170.4(4) . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.336 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.068