# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Zhiyong Wang' _publ_contact_author_email ZWANG3@USTC.EDU.CN _publ_section_title ; Influence of co-ligands and solvents on the packing and photoluminescence of three related MnII metal-organic frameworks ; loop_ _publ_author_name 'Zhiyong Wang.' 'Lexin Song.' 'Sujing Wang.' 'Shunshun Xiong.' # Attachment 'B817418Kcompound1revised.CIF' data_1a _database_code_depnum_ccdc_archive 'CCDC 688344' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H8 Mn N0 O5 S4' _chemical_formula_weight 415.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 '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 7.4040(15) _cell_length_b 26.670(5) _cell_length_c 8.2180(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.20(3) _cell_angle_gamma 90.00 _cell_volume 1601.9(6) _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 block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 11.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1264 _exptl_absorpt_correction_T_max 0.3860 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Gemini S Ultra' _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 7056 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 62.72 _reflns_number_total 2486 _reflns_number_gt 2084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis RED' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution ? _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^)+(0.0503P)^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 SHELXL _refine_ls_extinction_coef 0.00057(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2486 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Mn2 Mn 0.5000 0.5000 0.5000 0.01897(15) Uani 1 2 d S . . Mn1 Mn 0.0000 0.5000 0.5000 0.01981(15) Uani 1 2 d S . . S4 S 0.15378(8) 0.50404(2) 0.16059(7) 0.03242(18) Uani 1 1 d . . . S3 S 0.60750(10) 0.24237(3) 0.71493(13) 0.0636(3) Uani 1 1 d . . . S2 S 0.11336(9) 0.17900(2) 0.79647(9) 0.0412(2) Uani 1 1 d . . . S1 S 0.12800(9) 0.32443(2) 0.72155(9) 0.0420(2) Uani 1 1 d . . . O5 O 0.2248(2) 0.49862(6) 0.34541(18) 0.0263(4) Uani 1 1 d . . . O4 O 0.0773(2) 0.06984(6) 0.8859(2) 0.0341(4) Uani 1 1 d . . . O3 O 0.3464(2) 0.04632(6) 0.82008(18) 0.0281(4) Uani 1 1 d . . . O2 O 0.3917(2) 0.44913(6) 0.66044(19) 0.0280(4) Uani 1 1 d . . . O1 O 0.0918(2) 0.43276(6) 0.6344(2) 0.0321(4) Uani 1 1 d . . . H12C H 0.2810 0.4738 -0.0542 0.089 Uiso 1 1 calc R . . H12B H 0.4284 0.4762 0.1054 0.089 Uiso 1 1 calc R . . H12A H 0.2846 0.4326 0.0822 0.089 Uiso 1 1 calc R . . H11C H 0.3466 0.5701 0.1454 0.073 Uiso 1 1 calc R . . H11B H 0.1977 0.5682 -0.0132 0.073 Uiso 1 1 calc R . . H11A H 0.1481 0.5897 0.1516 0.073 Uiso 1 1 calc R . . H8 H 0.541(4) 0.1274(11) 0.775(3) 0.041(8) Uiso 1 1 d . . . H3 H 0.559(4) 0.3596(13) 0.660(4) 0.056(9) Uiso 1 1 d . . . C12 C 0.3042(5) 0.46745(14) 0.0622(3) 0.0594(9) Uani 1 1 d . . . C11 C 0.2191(4) 0.56501(12) 0.1047(3) 0.0488(7) Uani 1 1 d . . . C10 C 0.2278(3) 0.07860(8) 0.8394(3) 0.0241(5) Uani 1 1 d . . . C9 C 0.2731(3) 0.13109(8) 0.8028(3) 0.0287(5) Uani 1 1 d . . . C8 C 0.4393(4) 0.14775(9) 0.7774(4) 0.0381(6) Uani 1 1 d . . . C7 C 0.4405(4) 0.20001(9) 0.7520(4) 0.0405(7) Uani 1 1 d . . . C6 C 0.2731(4) 0.22243(9) 0.7578(3) 0.0356(6) Uani 1 1 d . . . C5 C 0.2788(4) 0.27513(9) 0.7330(3) 0.0353(6) Uani 1 1 d . . . C4 C 0.4511(4) 0.29113(10) 0.7090(4) 0.0404(7) Uani 1 1 d . . . C3 C 0.4611(4) 0.34307(9) 0.6832(3) 0.0372(6) Uani 1 1 d . . . C2 C 0.2987(3) 0.36601(8) 0.6873(3) 0.0293(5) Uani 1 1 d . . . C1 C 0.2573(3) 0.42002(8) 0.6579(3) 0.0237(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 Mn2 0.0214(3) 0.0127(3) 0.0230(3) 0.00014(18) 0.0041(2) -0.00051(19) Mn1 0.0241(3) 0.0124(3) 0.0239(3) 0.00014(18) 0.0068(2) -0.00083(19) S4 0.0292(4) 0.0482(4) 0.0194(3) 0.0011(2) 0.0023(2) -0.0055(3) S3 0.0430(5) 0.0184(3) 0.1377(8) 0.0164(4) 0.0395(5) 0.0053(3) S2 0.0396(4) 0.0153(3) 0.0730(5) 0.0107(3) 0.0227(3) 0.0033(3) S1 0.0381(4) 0.0148(3) 0.0766(5) 0.0107(3) 0.0201(3) 0.0033(3) O5 0.0233(9) 0.0393(10) 0.0164(8) 0.0021(6) 0.0035(6) -0.0005(7) O4 0.0384(10) 0.0186(8) 0.0482(10) 0.0077(7) 0.0160(8) 0.0012(7) O3 0.0377(10) 0.0147(8) 0.0328(9) 0.0045(6) 0.0092(7) 0.0078(7) O2 0.0353(9) 0.0156(8) 0.0342(9) 0.0051(6) 0.0087(7) -0.0029(7) O1 0.0333(10) 0.0176(8) 0.0457(10) 0.0075(7) 0.0069(8) 0.0015(7) C12 0.068(2) 0.078(2) 0.0342(15) -0.0131(16) 0.0156(15) 0.0059(19) C11 0.0543(19) 0.0544(18) 0.0368(14) 0.0153(13) 0.0041(13) -0.0024(15) C10 0.0350(14) 0.0151(11) 0.0214(11) 0.0030(9) 0.0022(10) -0.0015(10) C9 0.0377(14) 0.0148(11) 0.0353(13) 0.0039(9) 0.0114(11) 0.0034(10) C8 0.0406(16) 0.0156(12) 0.0612(18) 0.0060(11) 0.0172(13) 0.0043(12) C7 0.0388(16) 0.0175(12) 0.0684(18) 0.0078(12) 0.0180(13) 0.0019(11) C6 0.0403(15) 0.0161(12) 0.0540(16) 0.0077(10) 0.0182(12) 0.0032(11) C5 0.0388(15) 0.0156(12) 0.0545(16) 0.0083(11) 0.0164(13) 0.0043(11) C4 0.0376(16) 0.0187(13) 0.0685(18) 0.0073(12) 0.0194(13) 0.0038(11) C3 0.0386(16) 0.0174(13) 0.0583(17) 0.0064(11) 0.0163(13) 0.0007(12) C2 0.0360(15) 0.0158(11) 0.0375(13) 0.0046(10) 0.0101(11) 0.0003(10) C1 0.0372(15) 0.0148(11) 0.0202(11) 0.0030(8) 0.0080(10) 0.0008(11) _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 Mn2 O5 2.2222(17) 3_666 ? Mn2 O5 2.2222(17) . ? Mn2 O4 2.2018(16) 4_665 ? Mn2 O4 2.2018(16) 2_556 ? Mn2 O2 2.1355(15) 3_666 ? Mn2 O2 2.1355(15) . ? Mn1 O5 2.2500(16) 3_566 ? Mn1 O5 2.2500(16) . ? Mn1 O3 2.1138(15) 4_565 ? Mn1 O3 2.1138(15) 2_556 ? Mn1 O1 2.1582(16) 3_566 ? Mn1 O1 2.1582(16) . ? S4 O5 1.5326(16) . ? S4 C12 1.770(3) . ? S4 C11 1.778(3) . ? S3 C7 1.737(3) . ? S3 C4 1.737(3) . ? S2 C9 1.736(2) . ? S2 C6 1.721(3) . ? S1 C5 1.718(2) . ? S1 C2 1.738(2) . ? O4 Mn2 2.2018(16) 2_546 ? O4 C10 1.256(3) . ? O3 Mn1 2.1138(15) 2_546 ? O3 C10 1.258(3) . ? O2 C1 1.259(3) . ? O1 C1 1.257(3) . ? C9 C10 1.482(3) . ? C8 C9 1.355(4) . ? C7 C8 1.410(4) . ? C7 C6 1.384(4) . ? C6 C5 1.422(3) . ? C4 C5 1.389(4) . ? C4 C3 1.405(4) . ? C2 C3 1.354(4) . ? C2 C1 1.484(3) . ? 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 Mn2 O5 Mn1 111.74(6) . . ? S4 O5 Mn2 134.67(9) . . ? S4 O5 Mn1 112.97(9) . . ? O5 S4 C12 105.03(13) . . ? O5 S4 C11 106.14(11) . . ? O5 Mn2 O5 180 . 3_666 ? O5 Mn1 O5 180 . 3_566 ? O4 Mn2 O5 91.13(6) 4_665 . ? O4 Mn2 O5 91.13(6) 2_556 3_666 ? O4 Mn2 O5 88.87(6) 4_665 3_666 ? O4 Mn2 O5 88.87(6) 2_556 . ? O4 Mn2 O4 180 2_556 4_665 ? O4 C10 O3 125.6(2) . . ? O4 C10 C9 118.6(2) . . ? O3 Mn1 O5 92.32(6) 4_565 3_566 ? O3 Mn1 O5 92.32(6) 2_556 . ? O3 Mn1 O5 87.68(6) 4_565 . ? O3 Mn1 O5 87.68(6) 2_556 3_566 ? O3 Mn1 O3 180.00(7) 2_556 4_565 ? O3 Mn1 O1 92.14(6) 4_565 3_566 ? O3 Mn1 O1 92.14(6) 2_556 . ? O3 Mn1 O1 87.86(6) 4_565 . ? O3 Mn1 O1 87.86(6) 2_556 3_566 ? O3 C10 C9 115.8(2) . . ? O2 Mn2 O5 93.32(6) 3_666 . ? O2 Mn2 O5 93.32(6) . 3_666 ? O2 Mn2 O5 86.68(6) 3_666 3_666 ? O2 Mn2 O5 86.68(6) . . ? O2 Mn2 O4 97.22(6) 3_666 4_665 ? O2 Mn2 O4 97.22(6) . 2_556 ? O2 Mn2 O4 82.78(6) 3_666 2_556 ? O2 Mn2 O4 82.78(6) . 4_665 ? O2 Mn2 O2 180.00(6) 3_666 . ? O2 C1 C2 117.0(2) . . ? O1 Mn1 O5 94.28(6) 3_566 3_566 ? O1 Mn1 O5 94.28(6) . . ? O1 Mn1 O5 85.72(6) 3_566 . ? O1 Mn1 O5 85.72(6) . 3_566 ? O1 Mn1 O1 180.00(5) 3_566 . ? O1 C1 O2 125.7(2) . . ? O1 C1 C2 117.3(2) . . ? C12 S4 C11 99.75(16) . . ? C10 O4 Mn2 126.21(14) . 2_546 ? C10 O3 Mn1 128.32(14) . 2_546 ? C10 C9 S2 121.72(19) . . ? C9 C8 C7 112.0(2) . . ? C8 C9 S2 112.64(18) . . ? C8 C9 C10 125.6(2) . . ? C8 C7 S3 133.7(2) . . ? C7 C6 S2 111.18(18) . . ? C7 C6 C5 112.0(2) . . ? C6 S2 C9 90.91(12) . . ? C6 C7 S3 113.06(18) . . ? C6 C7 C8 113.3(2) . . ? C6 C5 S1 136.9(2) . . ? C5 S1 C2 90.81(12) . . ? C5 C6 S2 136.8(2) . . ? C5 C4 S3 112.92(18) . . ? C5 C4 C3 113.3(2) . . ? C4 S3 C7 90.11(13) . . ? C4 C5 S1 111.15(18) . . ? C4 C5 C6 111.9(2) . . ? C3 C4 S3 133.7(2) . . ? C3 C2 S1 112.78(18) . . ? C3 C2 C1 126.5(2) . . ? C2 C3 C4 111.9(2) . . ? C1 O2 Mn2 139.02(14) . . ? C1 O1 Mn1 121.53(14) . . ? C1 C2 S1 120.60(18) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 62.72 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.355 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.076 # Attachment 'B817418Kcompound3revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 688345' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H18 Mn2 N2 O11 S6' _chemical_formula_weight 836.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 '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/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 11.0311(4) _cell_length_b 11.5197(5) _cell_length_c 27.0330(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.739(4) _cell_angle_gamma 90.00 _cell_volume 3375.1(2) _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 block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 10.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2377 _exptl_absorpt_correction_T_max 0.4322 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Gemini S Ultra' _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 8414 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 62.81 _reflns_number_total 2652 _reflns_number_gt 2356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis RED' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution ? _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^)+(0.0621P)^2^+0.5882P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2652 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Mn1 Mn 0.91794(3) 0.12666(3) 1.002544(13) 0.02388(15) Uani 1 1 d . . . S3 S 0.47339(6) 0.37353(6) 0.68533(2) 0.03286(19) Uani 1 1 d . . . S2 S 0.57329(6) 0.29036(7) 0.82663(2) 0.0369(2) Uani 1 1 d . . . S1 S 0.83652(6) 0.44432(7) 0.75468(2) 0.0382(2) Uani 1 1 d . . . O6 O 1.07614(19) 0.2367(2) 1.01253(8) 0.0509(5) Uani 1 1 d . . . O5 O 0.7500 0.0150(2) 1.0000 0.0279(5) Uani 1 2 d S . . O4 O 0.62388(17) 0.20192(18) 0.93037(6) 0.0386(5) Uani 1 1 d . . . O3 O 0.82664(17) 0.23814(17) 0.94643(6) 0.0364(4) Uani 1 1 d . . . O2 O 0.35985(17) 0.42157(18) 0.58449(6) 0.0372(5) Uani 1 1 d . . . O1 O 0.52130(15) 0.48959(15) 0.55405(6) 0.0272(4) Uani 1 1 d . . . N1 N 1.1823 0.3528 1.0719 0.106 Uani 1 1 d . . . H13C H 1.1260 0.4498 1.0149 0.720 Uiso 1 1 calc R . . H13B H 1.0366 0.4447 1.0536 0.720 Uiso 1 1 calc R . . H13A H 1.1589 0.5169 1.0661 0.720 Uiso 1 1 calc R . . H12C H 1.2295 0.3357 1.1463 0.290 Uiso 1 1 calc R . . H12B H 1.3421 0.3267 1.1186 0.290 Uiso 1 1 calc R . . H12A H 1.2833 0.4481 1.1258 0.290 Uiso 1 1 calc R . . H11 H 1.1779 0.1917 1.0706 0.089 Uiso 1 1 calc R . . H8 H 0.7185 0.4997 0.6396 0.036 Uiso 1 1 calc R . . H3 H 0.8867 0.3483 0.8664 0.038 Uiso 1 1 calc R . . C13 C 1.1215 0.4481 1.0500 0.480 Uani 1 1 d . . . C12 C 1.2664 0.3670 1.1197 0.193 Uani 1 1 d . . . C11 C 1.1464(4) 0.2569(3) 1.05222(18) 0.0745(12) Uani 1 1 d . . . C10 C 0.4701(2) 0.4495(2) 0.58960(8) 0.0271(6) Uani 1 1 d . . . C9 C 0.5464(2) 0.4372(2) 0.64022(9) 0.0283(6) Uani 1 1 d . . . C8 C 0.6657(2) 0.4657(2) 0.65852(9) 0.0300(6) Uani 1 1 d . . . C7 C 0.6044(2) 0.3876(2) 0.72995(9) 0.0302(6) Uani 1 1 d . . . C6 C 0.6995(2) 0.4367(2) 0.71041(9) 0.0308(6) Uani 1 1 d . . . C5 C 0.6416(2) 0.3552(2) 0.78135(9) 0.0306(6) Uani 1 1 d . . . C4 C 0.7643(3) 0.3777(2) 0.79935(9) 0.0314(6) Uani 1 1 d . . . C3 C 0.8060(2) 0.3408(2) 0.84908(9) 0.0315(6) Uani 1 1 d . . . C2 C 0.7130(2) 0.2927(2) 0.86855(9) 0.0303(6) Uani 1 1 d . . . C1 C 0.7214(2) 0.2396(2) 0.91933(9) 0.0291(6) 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 0.0270(2) 0.0279(2) 0.0162(2) 0.00046(15) 0.00253(16) 0.00163(16) S3 0.0289(3) 0.0515(4) 0.0175(3) 0.0064(3) 0.0024(2) -0.0004(3) S2 0.0340(4) 0.0570(5) 0.0189(3) 0.0106(3) 0.0033(3) -0.0042(3) S1 0.0344(4) 0.0562(5) 0.0221(3) 0.0113(3) 0.0001(3) -0.0099(3) O6 0.0447(12) 0.0559(14) 0.0509(13) -0.0083(11) 0.0056(10) -0.0184(11) O5 0.0297(13) 0.0292(13) 0.0236(12) 0.000 0.0021(10) 0.000 O4 0.0419(11) 0.0506(12) 0.0230(9) 0.0106(8) 0.0053(8) -0.0036(9) O3 0.0404(11) 0.0423(11) 0.0238(9) 0.0105(8) -0.0013(8) 0.0011(9) O2 0.0336(10) 0.0548(13) 0.0218(9) 0.0102(8) 0.0017(7) -0.0018(9) O1 0.0330(9) 0.0344(10) 0.0146(8) 0.0041(7) 0.0052(7) 0.0055(8) N1 0.128 0.050 0.113 -0.026 -0.050 0.001 C13 0.788 0.065 0.386 -0.020 -0.415 0.019 C12 0.194 0.095 0.222 -0.063 -0.141 0.018 C11 0.059(2) 0.049(2) 0.102(3) -0.022(2) -0.021(2) 0.0122(18) C10 0.0324(14) 0.0307(13) 0.0185(12) 0.0009(10) 0.0054(10) 0.0072(11) C9 0.0329(13) 0.0357(14) 0.0171(11) 0.0041(10) 0.0064(10) 0.0064(11) C8 0.0344(14) 0.0362(14) 0.0196(12) 0.0050(10) 0.0052(10) -0.0009(11) C7 0.0327(14) 0.0392(15) 0.0177(12) 0.0043(10) 0.0022(10) 0.0016(12) C6 0.0341(14) 0.0372(14) 0.0197(12) 0.0044(10) 0.0017(10) -0.0016(12) C5 0.0335(14) 0.0405(15) 0.0172(12) 0.0056(10) 0.0033(10) 0.0000(12) C4 0.0354(14) 0.0386(15) 0.0196(13) 0.0062(10) 0.0033(11) 0.0000(12) C3 0.0342(14) 0.0367(14) 0.0213(12) 0.0039(11) -0.0006(10) 0.0004(12) C2 0.0364(14) 0.0352(14) 0.0174(12) 0.0052(10) 0.0004(10) 0.0038(12) C1 0.0429(16) 0.0265(13) 0.0169(12) 0.0027(10) 0.0028(11) 0.0037(12) _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 O6 2.133(2) . ? Mn1 O5 2.2457(14) . ? Mn1 O4 2.1366(18) 2_657 ? Mn1 O3 2.0966(17) . ? Mn1 O1 2.2673(16) 3_545 ? Mn1 O1 2.2283(17) 7_656 ? S3 C9 1.744(2) . ? S3 C7 1.709(3) . ? S2 C5 1.723(3) . ? S2 C2 1.735(3) . ? S1 C6 1.746(3) . ? S1 C4 1.744(3) . ? O6 C11 1.223(4) . ? O5 Mn1 2.2457(14) 2_657 ? O4 Mn1 2.1366(18) 2_657 ? O4 C1 1.247(3) . ? O3 C1 1.252(3) . ? O2 C10 1.240(3) . ? O1 Mn1 2.2672(16) 3_454 ? O1 Mn1 2.2283(17) 7_656 ? O1 C10 1.288(3) . ? N1 C13 1.3626 . ? N1 C12 1.4531 . ? N1 C11 1.258(4) . ? C10 C9 1.474(3) . ? C8 C9 1.357(4) . ? C8 C6 1.422(3) . ? C7 C6 1.380(4) . ? C5 C7 1.424(3) . ? C5 C4 1.375(4) . ? C3 C4 1.403(4) . ? C3 C2 1.355(4) . ? C2 C1 1.490(3) . ? 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 Mn1 O5 Mn1 110.13(10) . 2_657 ? Mn1 O1 Mn1 100.26(6) 7_656 3_454 ? O6 Mn1 O5 174.28(6) . . ? O6 Mn1 O4 87.27(8) . 2_657 ? O6 Mn1 O1 95.76(8) . 7_656 ? O6 Mn1 O1 91.73(8) . 3_545 ? O6 C11 N1 129.5(4) . . ? O5 Mn1 O1 86.42(6) . 3_545 ? O4 Mn1 O5 87.19(6) 2_657 . ? O4 Mn1 O1 85.68(7) 2_657 3_545 ? O4 Mn1 O1 165.19(7) 2_657 7_656 ? O4 C1 O3 127.0(2) . . ? O4 C1 C2 117.1(2) . . ? O3 Mn1 O6 89.94(8) . . ? O3 Mn1 O5 92.65(7) . . ? O3 Mn1 O4 102.42(8) . 2_657 ? O3 Mn1 O1 92.10(7) . 7_656 ? O3 Mn1 O1 171.80(7) . 3_545 ? O3 C1 C2 115.9(2) . . ? O2 C10 O1 124.6(2) . . ? O2 C10 C9 117.2(2) . . ? O1 Mn1 O5 89.24(6) 7_656 . ? O1 Mn1 O1 79.74(6) 7_656 3_545 ? O1 C10 C9 118.2(2) . . ? C13 N1 C12 118.438(2) . . ? C11 O6 Mn1 126.4(3) . . ? C11 N1 C13 115.72(18) . . ? C11 N1 C12 124.98(19) . . ? C10 O1 Mn1 121.78(16) . 7_656 ? C10 O1 Mn1 117.88(15) . 3_454 ? C10 C9 S3 115.54(19) . . ? C9 C8 C6 111.2(2) . . ? C8 C9 S3 112.95(18) . . ? C8 C9 C10 131.5(2) . . ? C8 C6 S1 134.3(2) . . ? C7 S3 C9 90.76(12) . . ? C7 C6 S1 112.38(19) . . ? C7 C6 C8 113.3(2) . . ? C7 C5 S2 136.3(2) . . ? C6 C7 S3 111.85(19) . . ? C6 C7 C5 112.3(2) . . ? C5 S2 C2 90.25(12) . . ? C5 C7 S3 135.7(2) . . ? C5 C4 S1 112.61(19) . . ? C5 C4 C3 114.0(2) . . ? C4 S1 C6 90.21(12) . . ? C4 C5 S2 111.24(19) . . ? C4 C5 C7 112.4(2) . . ? C3 C4 S1 133.3(2) . . ? C3 C2 S2 113.40(19) . . ? C3 C2 C1 127.2(2) . . ? C2 C3 C4 111.1(2) . . ? C1 O4 Mn1 132.60(16) . 2_657 ? C1 O3 Mn1 134.41(17) . . ? C1 C2 S2 119.4(2) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 62.81 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.784 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.062 # Attachment 'B817418Kcompound2revised.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 688346' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H13 Mn N2 O5 S3' _chemical_formula_weight 488.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.1491(3) _cell_length_b 7.65480(10) _cell_length_c 25.6413(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3954.85(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 8.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1800 _exptl_absorpt_correction_T_max 0.2751 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Gemini S Ultra' _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 9836 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 62.76 _reflns_number_total 3113 _reflns_number_gt 2580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis RED' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution ? _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^)+(0.0604P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00020(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3113 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.180562(18) 0.25885(5) 0.159881(14) 0.02528(14) Uani 1 1 d . . . S3 S 0.25946(3) 0.34375(9) -0.16568(2) 0.03085(18) Uani 1 1 d . . . S2 S 0.41389(3) 0.61137(10) -0.09147(2) 0.03735(19) Uani 1 1 d . . . S1 S 0.26248(3) 0.34467(9) -0.01290(2) 0.03174(18) Uani 1 1 d . . . O5 O 0.09034(9) 0.1760(3) 0.20886(7) 0.0430(5) Uani 1 1 d . . . O4 O 0.32373(8) 0.4844(2) -0.30387(6) 0.0336(4) Uani 1 1 d . . . O3 O 0.23943(8) 0.3177(3) -0.27631(7) 0.0385(4) Uani 1 1 d . . . O2 O 0.24933(9) 0.3203(3) 0.09971(6) 0.0378(4) Uani 1 1 d . . . O1 O 0.33016(8) 0.5056(2) 0.12251(6) 0.0350(4) Uani 1 1 d . . . N2 N 0.06036(11) 0.0424(3) 0.28428(9) 0.0428(6) Uani 1 1 d . . . N1 N 0.10130(11) 0.3705(3) 0.10622(9) 0.0353(5) Uani 1 1 d . . . H18C H 0.1192 -0.0396 0.3413 0.102 Uiso 1 1 calc R . . H18B H 0.0441 -0.0804 0.3513 0.102 Uiso 1 1 calc R . . H18A H 0.0845 -0.1924 0.3112 0.102 Uiso 1 1 calc R . . H17C H 0.0064 0.2591 0.2915 0.092 Uiso 1 1 calc R . . H17B H -0.0301 0.1109 0.2605 0.092 Uiso 1 1 calc R . . H17A H -0.0238 0.0991 0.3213 0.092 Uiso 1 1 calc R . . H16 H 0.1381 0.0018 0.2422 0.051 Uiso 1 1 calc R . . H14 H 0.0913 0.6588 0.0161 0.090 Uiso 1 1 calc R . . H13 H -0.0335 0.2687 0.0467 0.039 Uiso 1 1 calc R . . H12 H 0.0347 0.1887 0.1137 0.040 Uiso 1 1 calc R . . H11 H 0.1524 0.5749 0.0868 0.080 Uiso 1 1 calc R . . H8 H 0.3931 0.5828 -0.2143 0.033 Uiso 1 1 calc R . . H3 H 0.3977 0.5870 0.0314 0.038 Uiso 1 1 calc R . . C18 C 0.07857(18) -0.0776(5) 0.32548(13) 0.0683(10) Uani 1 1 d . . . C17 C -0.00212(15) 0.1358(5) 0.28988(13) 0.0612(9) Uani 1 1 d . . . C16 C 0.09982(14) 0.0692(4) 0.24414(11) 0.0422(7) Uani 1 1 d . . . C15 C 0.02074(12) 0.4738(4) 0.02274(11) 0.0381(6) Uani 1 1 d . . . C14 C 0.07793(16) 0.5629(4) 0.03571(15) 0.0752(13) Uani 1 1 d . . . C13 C 0.00484(12) 0.3324(3) 0.05333(10) 0.0328(6) Uani 1 1 d . . . C12 C 0.04620(12) 0.2857(4) 0.09386(9) 0.0331(6) Uani 1 1 d . . . C11 C 0.11525(18) 0.5093(5) 0.07789(14) 0.0666(11) Uani 1 1 d . . . C10 C 0.28953(11) 0.4123(3) -0.26937(9) 0.0282(5) Uani 1 1 d . . . C9 C 0.30890(11) 0.4366(3) -0.21382(9) 0.0279(5) Uani 1 1 d . . . C8 C 0.36150(11) 0.5258(3) -0.19405(9) 0.0275(5) Uani 1 1 d . . . C7 C 0.36219(11) 0.5213(3) -0.13919(9) 0.0281(5) Uani 1 1 d . . . C6 C 0.31011(11) 0.4276(3) -0.11772(9) 0.0264(5) Uani 1 1 d . . . C5 C 0.31098(11) 0.4275(3) -0.06240(9) 0.0270(5) Uani 1 1 d . . . C4 C 0.36395(11) 0.5221(3) -0.04271(9) 0.0282(5) Uani 1 1 d . . . C3 C 0.36528(12) 0.5291(3) 0.01219(9) 0.0313(6) Uani 1 1 d . . . C2 C 0.31338(11) 0.4408(3) 0.03374(9) 0.0277(5) Uani 1 1 d . . . C1 C 0.29627(13) 0.4218(3) 0.09026(9) 0.0284(6) 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 0.0273(2) 0.0350(2) 0.0136(2) 0.00074(16) -0.00107(15) 0.00114(17) S3 0.0337(3) 0.0417(4) 0.0171(3) 0.0002(3) -0.0019(3) -0.0115(3) S2 0.0392(4) 0.0532(4) 0.0197(3) 0.0005(3) -0.0004(3) -0.0203(3) S1 0.0368(3) 0.0408(3) 0.0176(3) 0.0003(3) 0.0021(3) -0.0115(3) O5 0.0453(10) 0.0535(12) 0.0301(10) 0.0048(10) 0.0065(9) -0.0039(9) O4 0.0419(9) 0.0393(10) 0.0196(9) 0.0042(8) 0.0049(8) 0.0005(8) O3 0.0407(10) 0.0559(11) 0.0188(9) 0.0003(8) -0.0063(8) -0.0132(9) O2 0.0438(10) 0.0490(11) 0.0207(9) -0.0006(8) 0.0088(8) -0.0091(9) O1 0.0475(10) 0.0385(10) 0.0190(9) -0.0040(8) -0.0041(8) 0.0011(9) N2 0.0398(12) 0.0499(14) 0.0387(13) 0.0053(11) 0.0097(11) -0.0036(11) N1 0.0389(12) 0.0383(13) 0.0286(11) -0.0007(10) -0.0107(10) 0.0031(10) C18 0.077(2) 0.068(2) 0.060(2) 0.0296(18) 0.0193(19) 0.000(2) C17 0.0422(15) 0.084(3) 0.057(2) 0.0022(19) 0.0124(16) -0.0011(16) C16 0.0426(14) 0.0417(16) 0.0424(17) -0.0015(14) 0.0102(14) -0.0050(13) C15 0.0361(13) 0.0404(15) 0.0378(15) 0.0006(12) -0.0135(12) 0.0039(12) C14 0.071(2) 0.056(2) 0.098(3) 0.041(2) -0.059(2) -0.0300(18) C13 0.0266(12) 0.0446(15) 0.0272(14) 0.0008(12) -0.0031(11) -0.0010(11) C12 0.0298(13) 0.0449(15) 0.0247(14) 0.0019(11) 0.0037(11) 0.0016(12) C11 0.067(2) 0.0513(19) 0.082(3) 0.0271(19) -0.0469(19) -0.0229(17) C10 0.0330(12) 0.0316(13) 0.0201(13) -0.0012(11) -0.0009(11) 0.0038(11) C9 0.0330(12) 0.0333(13) 0.0175(12) 0.0025(10) 0.0019(10) -0.0011(11) C8 0.0302(12) 0.0336(13) 0.0189(12) 0.0027(10) 0.0039(10) -0.0034(11) C7 0.0314(12) 0.0315(13) 0.0212(13) -0.0016(10) -0.0014(10) -0.0060(11) C6 0.0299(12) 0.0319(13) 0.0174(12) -0.0012(10) -0.0011(10) -0.0050(11) C5 0.0307(12) 0.0325(13) 0.0179(13) -0.0001(10) 0.0029(10) -0.0043(11) C4 0.0321(12) 0.0336(13) 0.0190(12) 0.0000(10) 0.0016(11) -0.0061(11) C3 0.0369(13) 0.0374(14) 0.0194(13) -0.0028(11) -0.0034(11) -0.0083(12) C2 0.0355(13) 0.0300(13) 0.0177(13) -0.0034(10) -0.0005(10) -0.0006(11) C1 0.0338(13) 0.0304(13) 0.0211(13) 0.0003(11) 0.0015(11) 0.0065(11) _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 O5 2.2988(18) . ? Mn1 O4 2.1759(17) 2_565 ? Mn1 O3 2.1041(17) 8_566 ? Mn1 O2 2.1264(17) . ? Mn1 O1 2.1736(18) 7_655 ? Mn1 N1 2.275(2) . ? S3 C9 1.738(2) . ? S3 C6 1.722(2) . ? S2 C7 1.749(2) . ? S2 C4 1.745(2) . ? S1 C5 1.723(2) . ? S1 C2 1.739(2) . ? O5 C16 1.234(3) . ? O4 Mn1 2.1759(17) 2_564 ? O4 C10 1.250(3) . ? O3 Mn1 2.1041(17) 8_565 ? O3 C10 1.255(3) . ? O2 C1 1.248(3) . ? O1 Mn1 2.1736(17) 7_665 ? O1 C1 1.250(3) . ? N2 C18 1.447(4) . ? N2 C17 1.455(4) . ? N2 C16 1.317(3) . ? N1 C12 1.324(3) . ? N1 C11 1.318(4) . ? C15 C15 1.490(5) 5_565 ? C15 C14 1.380(4) . ? C13 C15 1.374(4) . ? C13 C12 1.379(3) . ? C11 C14 1.380(4) . ? C9 C8 1.359(3) . ? C9 C10 1.489(3) . ? C8 C7 1.407(3) . ? C7 C6 1.385(3) . ? C5 C6 1.418(3) . ? C5 C4 1.385(3) . ? C3 C4 1.409(3) . ? C3 C2 1.362(3) . ? C1 C2 1.497(3) . ? 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 O5 C16 N2 125.6(3) . . ? O4 Mn1 O5 89.11(7) 2_565 . ? O4 Mn1 N1 83.76(7) 2_565 . ? O4 C10 O3 126.7(2) . . ? O4 C10 C9 118.5(2) . . ? O3 Mn1 O5 86.79(7) 8_566 . ? O3 Mn1 O4 86.66(7) 8_566 2_565 ? O3 Mn1 O2 104.98(7) 8_566 . ? O3 Mn1 O1 98.65(7) 8_566 7_655 ? O3 Mn1 N1 166.12(7) 8_566 . ? O3 C10 C9 114.8(2) . . ? O2 Mn1 O5 166.60(7) . . ? O2 Mn1 O4 97.82(7) . 2_565 ? O2 Mn1 O1 86.69(7) . 7_655 ? O2 Mn1 N1 86.30(8) . . ? O2 C1 O1 127.2(2) . . ? O2 C1 C2 115.0(2) . . ? O1 Mn1 O5 85.18(7) 7_655 . ? O1 Mn1 O4 171.96(7) 7_655 2_565 ? O1 Mn1 N1 89.92(7) 7_655 . ? O1 C1 C2 117.7(2) . . ? N1 Mn1 O5 83.04(8) . . ? N1 C12 C13 124.0(2) . . ? N1 C11 C14 123.8(3) . . ? C18 N2 C17 117.3(2) . . ? C16 O5 Mn1 117.45(18) . . ? C16 N2 C18 121.1(3) . . ? C16 N2 C17 121.5(3) . . ? C15 C14 C11 119.8(3) . . ? C15 C13 C12 119.6(2) . . ? C14 C15 C15 121.6(3) . 5_565 ? C13 C15 C15 121.9(3) . 5_565 ? C13 C15 C14 116.5(2) . . ? C12 N1 Mn1 123.32(18) . . ? C11 N1 Mn1 119.11(19) . . ? C11 N1 C12 116.2(2) . . ? C10 O4 Mn1 132.81(16) . 2_564 ? C10 O3 Mn1 136.42(16) . 8_565 ? C10 C9 S3 118.57(17) . . ? C9 C8 C7 111.6(2) . . ? C8 C9 S3 112.81(18) . . ? C8 C9 C10 128.6(2) . . ? C8 C7 S2 134.07(18) . . ? C7 C6 S3 110.97(17) . . ? C7 C6 C5 112.9(2) . . ? C6 S3 C9 90.87(11) . . ? C6 C7 S2 112.17(17) . . ? C6 C7 C8 113.8(2) . . ? C6 C5 S1 136.88(17) . . ? C5 S1 C2 90.95(11) . . ? C5 C6 S3 136.15(17) . . ? C5 C4 S2 112.83(18) . . ? C5 C4 C3 113.5(2) . . ? C4 S2 C7 90.19(11) . . ? C4 C5 S1 111.15(18) . . ? C4 C5 C6 111.9(2) . . ? C3 C4 S2 133.65(18) . . ? C3 C2 S1 112.56(18) . . ? C3 C2 C1 128.2(2) . . ? C2 C3 C4 111.8(2) . . ? C1 O2 Mn1 140.59(16) . . ? C1 O1 Mn1 134.04(16) . 7_665 ? C1 C2 S1 119.28(18) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 62.76 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.356 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.056