# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Xiao-Ming Chen' _publ_contact_author_email CXM@MAIL.SYSU.EDU.CN _publ_section_title ; Two spin-competing manganese(II) coordination polymers exhibiting unusual multi-step magnetization jumps ; loop_ _publ_author_name 'Xiao-Ming Chen' 'Wei Xue' 'Wei-Xiong Zhang' 'Yan-Zhen Zheng' # Attachment '1.cif' data_mn _database_code_depnum_ccdc_archive 'CCDC 724458' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 Mn3 N8 O10' _chemical_formula_weight 543.06 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2934(14) _cell_length_b 9.4532(10) _cell_length_c 7.2959(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.465(2) _cell_angle_gamma 90.00 _cell_volume 836.33(16) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1279 _cell_measurement_theta_min 2.732 _cell_measurement_theta_max 27.705 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 2.305 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7537 _exptl_absorpt_correction_T_max 0.9134 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _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 4014 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1623 _reflns_number_gt 1371 _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^)+(0.0429P)^2^+1.0588P] 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 1623 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 1.0000 0.5000 0.0000 0.0228(2) Uani 1 2 d S . . Mn2 Mn 1.38431(4) 0.49956(4) 0.61323(6) 0.01708(16) Uani 1 1 d . . . O1 O 1.13521(19) 0.3851(2) 0.1712(3) 0.0292(6) Uani 1 1 d . . . O2 O 1.28523(19) 0.4063(2) 0.3817(3) 0.0260(5) Uani 1 1 d . . . O3 O 1.46435(17) 0.6144(2) 0.4016(3) 0.0204(5) Uani 1 1 d . . . O4 O 1.46795(18) 0.8375(2) 0.3069(3) 0.0250(5) Uani 1 1 d . . . N1 N 1.1382(2) 0.6584(3) 0.0734(3) 0.0189(6) Uani 1 1 d . . . N2 N 1.1587(2) 0.7939(3) 0.0408(3) 0.0194(6) Uani 1 1 d . . . N3 N 1.2609(2) 0.8251(3) 0.1244(3) 0.0181(6) Uani 1 1 d . . . C1 C 1.2162(3) 0.4539(3) 0.2506(4) 0.0200(7) Uani 1 1 d . . . C2 C 1.2271(2) 0.6020(3) 0.1827(4) 0.0167(6) Uani 1 1 d . . . C3 C 1.3058(2) 0.7092(3) 0.2138(4) 0.0157(6) Uani 1 1 d . . . C4 C 1.4203(2) 0.7217(3) 0.3140(4) 0.0164(6) Uani 1 1 d . . . O1W O 1.3510(2) 0.3827(3) 0.8563(4) 0.0405(7) Uani 1 1 d . . . H1A H 1.3275 0.2980 0.8546 0.061 Uiso 1 1 d R . . H1B H 1.4025 0.3843 0.9496 0.061 Uiso 1 1 d R . . N4 N 1.0570(3) 0.4260(3) -0.2636(4) 0.0342(7) Uani 1 1 d . . . H4A H 1.0113 0.3595 -0.3176 0.051 Uiso 1 1 calc R . . H4B H 1.1247 0.3905 -0.2361 0.051 Uiso 1 1 calc R . . H4C H 1.0572 0.4988 -0.3409 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0183(4) 0.0230(4) 0.0241(4) 0.0014(3) -0.0052(3) -0.0053(3) Mn2 0.0158(3) 0.0137(3) 0.0207(3) -0.00089(18) 0.00002(19) 0.00153(18) O1 0.0280(13) 0.0169(12) 0.0370(14) 0.0044(10) -0.0113(11) -0.0076(10) O2 0.0302(13) 0.0143(11) 0.0284(12) 0.0014(9) -0.0101(10) -0.0013(10) O3 0.0153(11) 0.0184(11) 0.0268(12) 0.0071(9) 0.0018(9) 0.0033(9) O4 0.0188(12) 0.0193(12) 0.0335(13) 0.0080(10) -0.0058(9) -0.0045(9) N1 0.0172(13) 0.0171(13) 0.0212(13) 0.0022(10) -0.0007(10) -0.0020(11) N2 0.0160(13) 0.0189(13) 0.0219(13) 0.0034(11) -0.0011(10) -0.0007(11) N3 0.0135(13) 0.0191(13) 0.0201(13) 0.0033(10) -0.0018(10) -0.0003(11) C1 0.0214(17) 0.0168(15) 0.0217(16) -0.0005(13) 0.0033(13) -0.0010(13) C2 0.0148(15) 0.0163(15) 0.0184(15) 0.0000(12) 0.0008(12) -0.0007(12) C3 0.0161(16) 0.0148(15) 0.0161(14) 0.0009(12) 0.0024(12) 0.0016(12) C4 0.0145(15) 0.0175(15) 0.0169(14) 0.0012(12) 0.0020(12) 0.0022(12) O1W 0.0466(17) 0.0362(15) 0.0373(15) 0.0056(12) 0.0022(12) -0.0091(13) N4 0.0345(18) 0.0325(17) 0.0361(17) 0.0001(14) 0.0072(14) -0.0006(14) _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 O1 2.195(2) 3_765 ? Mn1 O1 2.195(2) . ? Mn1 N1 2.262(2) . ? Mn1 N1 2.262(2) 3_765 ? Mn1 N4 2.263(3) . ? Mn1 N4 2.263(3) 3_765 ? Mn2 O2 2.107(2) . ? Mn2 O3 2.168(2) 3_866 ? Mn2 O1W 2.185(3) . ? Mn2 O4 2.225(2) 4_576 ? Mn2 O3 2.243(2) . ? Mn2 N3 2.258(2) 4_576 ? O1 C1 1.249(4) . ? O2 C1 1.253(4) . ? O3 C4 1.272(3) . ? O3 Mn2 2.168(2) 3_866 ? O4 C4 1.247(4) . ? O4 Mn2 2.225(2) 4_575 ? N1 N2 1.334(3) . ? N1 C2 1.352(4) . ? N2 N3 1.336(3) . ? N3 C3 1.346(4) . ? N3 Mn2 2.258(2) 4_575 ? C1 C2 1.499(4) . ? C2 C3 1.393(4) . ? C3 C4 1.480(4) . ? O1W H1A 0.8500 . ? O1W H1B 0.8500 . ? N4 H4A 0.8900 . ? N4 H4B 0.8900 . ? N4 H4C 0.8900 . ? 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 Mn1 O1 180.00(10) 3_765 . ? O1 Mn1 N1 106.02(8) 3_765 . ? O1 Mn1 N1 73.98(8) . . ? O1 Mn1 N1 73.98(8) 3_765 3_765 ? O1 Mn1 N1 106.02(8) . 3_765 ? N1 Mn1 N1 180.0 . 3_765 ? O1 Mn1 N4 88.89(10) 3_765 . ? O1 Mn1 N4 91.11(10) . . ? N1 Mn1 N4 94.62(10) . . ? N1 Mn1 N4 85.38(10) 3_765 . ? O1 Mn1 N4 91.11(10) 3_765 3_765 ? O1 Mn1 N4 88.89(10) . 3_765 ? N1 Mn1 N4 85.38(10) . 3_765 ? N1 Mn1 N4 94.62(10) 3_765 3_765 ? N4 Mn1 N4 180.00(14) . 3_765 ? O2 Mn2 O3 98.04(9) . 3_866 ? O2 Mn2 O1W 106.17(9) . . ? O3 Mn2 O1W 93.80(9) 3_866 . ? O2 Mn2 O4 160.91(8) . 4_576 ? O3 Mn2 O4 93.73(8) 3_866 4_576 ? O1W Mn2 O4 87.90(9) . 4_576 ? O2 Mn2 O3 84.94(8) . . ? O3 Mn2 O3 74.28(8) 3_866 . ? O1W Mn2 O3 164.95(9) . . ? O4 Mn2 O3 83.85(8) 4_576 . ? O2 Mn2 N3 91.87(9) . 4_576 ? O3 Mn2 N3 162.57(8) 3_866 4_576 ? O1W Mn2 N3 97.18(10) . 4_576 ? O4 Mn2 N3 73.27(8) 4_576 4_576 ? O3 Mn2 N3 92.47(8) . 4_576 ? C1 O1 Mn1 118.5(2) . . ? C1 O2 Mn2 133.8(2) . . ? C4 O3 Mn2 132.04(18) . 3_866 ? C4 O3 Mn2 122.21(18) . . ? Mn2 O3 Mn2 105.72(8) 3_866 . ? C4 O4 Mn2 117.57(19) . 4_575 ? N2 N1 C2 109.0(2) . . ? N2 N1 Mn1 138.6(2) . . ? C2 N1 Mn1 112.41(19) . . ? N1 N2 N3 108.8(2) . . ? N2 N3 C3 108.7(2) . . ? N2 N3 Mn2 137.12(19) . 4_575 ? C3 N3 Mn2 112.97(19) . 4_575 ? O1 C1 O2 123.7(3) . . ? O1 C1 C2 116.2(3) . . ? O2 C1 C2 120.1(3) . . ? N1 C2 C3 106.3(3) . . ? N1 C2 C1 117.1(3) . . ? C3 C2 C1 136.3(3) . . ? N3 C3 C2 107.1(2) . . ? N3 C3 C4 117.1(3) . . ? C2 C3 C4 135.8(3) . . ? O4 C4 O3 123.8(3) . . ? O4 C4 C3 117.7(3) . . ? O3 C4 C3 118.5(3) . . ? Mn2 O1W H1A 124.9 . . ? Mn2 O1W H1B 115.3 . . ? H1A O1W H1B 103.6 . . ? Mn1 N4 H4A 109.5 . . ? Mn1 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Mn1 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.371 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.086 # Attachment '2.cif' data_mn _database_code_depnum_ccdc_archive 'CCDC 724459' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H8 Mn3 N6 O12' _chemical_formula_weight 545.02 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5597(6) _cell_length_b 16.3583(13) _cell_length_c 13.0734(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.6520(10) _cell_angle_gamma 90.00 _cell_volume 1615.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2549 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.312 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 2.394 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6090 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _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 6982 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3087 _reflns_number_gt 2643 _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. In Checkcif report, the following ALERTS were generated PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... Z Author response: There is pseudo symmetry element, which is a local inversion centre between Mn1 and Mn2 atoms. ABSTY02_ALERT_1_C An _exptl_absorpt_correction_type has been given without a literature citation. This should be contained in the _exptl_absorpt_process_details field. Absorption correction given as empirical 029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 -- O3W .. 5.04 su 062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.17 Ratio ; _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^)+(0.0372P)^2^+0.5210P] 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 3087 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0752 _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 Mn1 Mn -0.12449(4) 0.44206(2) 0.83910(3) 0.01787(12) Uani 1 1 d . . . Mn2 Mn 0.11520(4) 0.55083(2) 0.66148(3) 0.01595(11) Uani 1 1 d . . . Mn3 Mn 0.61592(4) 0.747602(19) 0.41015(3) 0.01545(11) Uani 1 1 d . . . O1W O -0.2476(3) 0.44008(12) 0.97964(14) 0.0460(6) Uani 1 1 d . . . H1A H -0.3174 0.4059 1.0057 0.069 Uiso 1 1 d R . . H1B H -0.2308 0.4754 1.0267 0.069 Uiso 1 1 d R . . O1 O 0.0355(2) 0.42791(9) 0.69345(12) 0.0209(4) Uani 1 1 d . . . O2 O 0.1700(2) 0.34044(10) 0.59307(12) 0.0221(4) Uani 1 1 d . . . O2W O -0.3625(2) 0.44799(11) 0.74332(14) 0.0363(5) Uani 1 1 d . . . H2A H -0.3856 0.4194 0.6900 0.054 Uiso 1 1 d R . . H2B H -0.4550 0.4764 0.7511 0.054 Uiso 1 1 d R . . O3W O 0.1549(2) 0.42478(11) 0.91467(13) 0.0308(4) Uani 1 1 d . . . H3A H 0.1535 0.3970 0.9695 0.046 Uiso 1 1 d R . . H3B H 0.2268 0.3996 0.8777 0.046 Uiso 1 1 d R . . O3 O 0.1752(2) 0.15865(10) 0.59232(12) 0.0222(4) Uani 1 1 d . . . O4W O -0.1306(2) 0.55498(10) 0.57116(13) 0.0283(4) Uani 1 1 d . . . H4A H -0.1453 0.5901 0.5236 0.042 Uiso 1 1 d R . . H4B H -0.1935 0.5144 0.5512 0.042 Uiso 1 1 d R . . O4 O 0.0466(2) 0.06702(9) 0.69035(12) 0.0186(4) Uani 1 1 d . . . O5 O 0.4349(2) 0.64971(10) 0.88187(12) 0.0273(4) Uani 1 1 d . . . O6 O 0.3456(2) 0.55506(9) 0.76795(13) 0.0208(4) Uani 1 1 d . . . O7 O 0.2945(2) 0.56745(10) 0.54181(12) 0.0249(4) Uani 1 1 d . . . O8 O 0.4396(2) 0.64188(10) 0.43117(12) 0.0258(4) Uani 1 1 d . . . N1 N -0.0896(2) 0.31260(11) 0.81059(15) 0.0186(4) Uani 1 1 d . . . N2 N -0.1325(3) 0.24688(10) 0.86339(17) 0.0204(5) Uani 1 1 d . . . N3 N -0.0742(2) 0.18101(11) 0.81459(14) 0.0180(4) Uani 1 1 d . . . N4 N 0.5765(3) 0.74449(11) 0.74083(15) 0.0183(4) Uani 1 1 d . . . N5 N 0.6289(2) 0.78385(13) 0.65800(14) 0.0206(4) Uani 1 1 d . . . N6 N 0.5748(3) 0.74149(11) 0.57493(15) 0.0175(4) Uani 1 1 d . . . C1 C 0.0738(3) 0.35593(13) 0.66549(17) 0.0159(5) Uani 1 1 d . . . C2 C -0.0009(3) 0.28932(13) 0.72760(17) 0.0153(5) Uani 1 1 d . . . C3 C 0.0082(3) 0.20495(13) 0.73025(17) 0.0151(5) Uani 1 1 d . . . C4 C 0.0830(3) 0.13986(14) 0.66555(17) 0.0157(5) Uani 1 1 d . . . C5 C 0.4174(3) 0.62267(14) 0.79137(17) 0.0191(5) Uani 1 1 d . . . C6 C 0.4887(3) 0.67573(14) 0.71010(17) 0.0168(5) Uani 1 1 d . . . C7 C 0.4862(3) 0.67414(14) 0.60426(17) 0.0172(5) Uani 1 1 d . . . C8 C 0.4001(3) 0.62356(14) 0.52090(18) 0.0195(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 Mn1 0.0241(2) 0.01083(19) 0.0191(2) -0.00088(13) 0.00553(16) 0.00004(13) Mn2 0.0201(2) 0.01057(19) 0.0175(2) -0.00067(13) 0.00443(16) -0.00132(13) Mn3 0.0196(2) 0.0161(2) 0.0108(2) 0.00113(13) 0.00284(16) 0.00016(13) O1W 0.0681(14) 0.0400(12) 0.0323(12) -0.0100(9) 0.0292(11) -0.0235(10) O1 0.0304(9) 0.0100(8) 0.0229(9) 0.0015(7) 0.0081(7) -0.0001(7) O2 0.0288(9) 0.0172(8) 0.0211(9) 0.0056(7) 0.0098(7) 0.0054(7) O2W 0.0317(10) 0.0383(12) 0.0379(12) -0.0174(9) -0.0094(9) 0.0101(8) O3W 0.0367(10) 0.0305(10) 0.0250(10) 0.0026(8) -0.0022(8) 0.0027(8) O3 0.0298(9) 0.0183(9) 0.0194(9) -0.0041(7) 0.0103(7) -0.0073(7) O4W 0.0357(10) 0.0210(10) 0.0270(10) 0.0058(7) -0.0101(8) -0.0065(7) O4 0.0245(8) 0.0095(7) 0.0222(9) -0.0001(6) 0.0058(7) 0.0004(6) O5 0.0362(10) 0.0307(10) 0.0153(9) -0.0012(7) 0.0039(8) -0.0140(8) O6 0.0221(8) 0.0177(9) 0.0225(9) 0.0019(7) -0.0004(7) -0.0036(6) O7 0.0301(9) 0.0253(9) 0.0201(9) -0.0050(7) 0.0080(8) -0.0127(7) O8 0.0330(9) 0.0297(10) 0.0150(9) -0.0025(7) 0.0044(8) -0.0121(8) N1 0.0234(10) 0.0120(9) 0.0208(11) -0.0004(8) 0.0064(9) -0.0006(8) N2 0.0258(11) 0.0126(10) 0.0235(12) 0.0001(8) 0.0089(9) -0.0006(7) N3 0.0228(10) 0.0122(9) 0.0196(10) -0.0002(8) 0.0066(8) -0.0009(8) N4 0.0231(10) 0.0198(11) 0.0121(10) 0.0005(8) 0.0007(9) -0.0047(8) N5 0.0254(11) 0.0228(11) 0.0135(11) 0.0002(8) 0.0011(9) -0.0062(8) N6 0.0196(10) 0.0206(10) 0.0124(11) -0.0010(8) 0.0014(9) -0.0038(8) C1 0.0170(11) 0.0134(11) 0.0174(12) 0.0016(9) 0.0003(9) 0.0014(9) C2 0.0171(11) 0.0137(11) 0.0154(12) 0.0001(9) 0.0033(9) -0.0002(9) C3 0.0158(10) 0.0121(11) 0.0175(12) 0.0012(9) 0.0025(9) -0.0016(8) C4 0.0143(10) 0.0157(11) 0.0171(12) -0.0008(9) -0.0012(9) -0.0001(9) C5 0.0162(11) 0.0238(13) 0.0173(12) 0.0010(10) 0.0012(10) 0.0006(9) C6 0.0168(11) 0.0181(12) 0.0156(12) -0.0007(9) 0.0017(9) -0.0005(9) C7 0.0187(11) 0.0184(11) 0.0146(12) 0.0018(9) 0.0030(9) -0.0011(9) C8 0.0189(11) 0.0207(12) 0.0192(13) -0.0024(10) 0.0032(10) -0.0010(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 Mn1 O1W 2.0980(18) . ? Mn1 O2W 2.1465(18) . ? Mn1 O4 2.1666(15) 2_556 ? Mn1 N1 2.1685(18) . ? Mn1 O3W 2.3076(18) . ? Mn1 O1 2.3143(15) . ? Mn2 O7 2.1345(16) . ? Mn2 O1 2.1458(15) . ? Mn2 O4W 2.1564(17) . ? Mn2 N3 2.1766(18) 2_556 ? Mn2 O6 2.1799(16) . ? Mn2 O4 2.3532(15) 2_556 ? Mn3 O2 2.1681(16) 3_666 ? Mn3 O5 2.1871(16) 4_575 ? Mn3 N6 2.193(2) . ? Mn3 O3 2.2028(16) 3_666 ? Mn3 O8 2.2087(16) . ? Mn3 N4 2.224(2) 4_575 ? O1W H1A 0.8500 . ? O1W H1B 0.8499 . ? O1 C1 1.270(3) . ? O2 C1 1.246(3) . ? O2 Mn3 2.1681(16) 3_666 ? O2W H2A 0.8500 . ? O2W H2B 0.8500 . ? O3W H3A 0.8500 . ? O3W H3B 0.8500 . ? O3 C4 1.248(3) . ? O3 Mn3 2.2028(15) 3_666 ? O4W H4A 0.8499 . ? O4W H4B 0.8501 . ? O4 C4 1.268(3) . ? O4 Mn1 2.1666(15) 2_546 ? O4 Mn2 2.3532(15) 2_546 ? O5 C5 1.264(3) . ? O5 Mn3 2.1871(16) 4_576 ? O6 C5 1.263(3) . ? O7 C8 1.254(3) . ? O8 C8 1.260(3) . ? N1 N2 1.326(3) . ? N1 C2 1.356(3) . ? N2 N3 1.337(3) . ? N3 C3 1.349(3) . ? N3 Mn2 2.1766(18) 2_546 ? N4 N5 1.336(3) . ? N4 C6 1.357(3) . ? N4 Mn3 2.224(2) 4_576 ? N5 N6 1.336(3) . ? N6 C7 1.354(3) . ? C1 C2 1.486(3) . ? C2 C3 1.382(3) . ? C3 C4 1.488(3) . ? C5 C6 1.492(3) . ? C6 C7 1.383(3) . ? C7 C8 1.494(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 O1W Mn1 O2W 96.75(8) . . ? O1W Mn1 O4 107.79(7) . 2_556 ? O2W Mn1 O4 94.65(7) . 2_556 ? O1W Mn1 N1 101.41(7) . . ? O2W Mn1 N1 92.82(7) . . ? O4 Mn1 N1 148.71(6) 2_556 . ? O1W Mn1 O3W 93.31(8) . . ? O2W Mn1 O3W 168.94(7) . . ? O4 Mn1 O3W 86.60(6) 2_556 . ? N1 Mn1 O3W 80.66(7) . . ? O1W Mn1 O1 171.49(7) . . ? O2W Mn1 O1 88.88(7) . . ? O4 Mn1 O1 77.96(6) 2_556 . ? N1 Mn1 O1 71.85(6) . . ? O3W Mn1 O1 80.62(6) . . ? O7 Mn2 O1 117.11(6) . . ? O7 Mn2 O4W 98.93(7) . . ? O1 Mn2 O4W 83.89(6) . . ? O7 Mn2 N3 94.60(7) . 2_556 ? O1 Mn2 N3 147.75(6) . 2_556 ? O4W Mn2 N3 85.59(7) . 2_556 ? O7 Mn2 O6 87.03(6) . . ? O1 Mn2 O6 97.39(6) . . ? O4W Mn2 O6 172.58(6) . . ? N3 Mn2 O6 89.54(7) 2_556 . ? O7 Mn2 O4 163.94(6) . 2_556 ? O1 Mn2 O4 77.52(6) . 2_556 ? O4W Mn2 O4 88.83(6) . 2_556 ? N3 Mn2 O4 71.86(6) 2_556 2_556 ? O6 Mn2 O4 84.33(6) . 2_556 ? O2 Mn3 O5 165.59(6) 3_666 4_575 ? O2 Mn3 N6 97.38(7) 3_666 . ? O5 Mn3 N6 94.88(7) 4_575 . ? O2 Mn3 O3 85.75(7) 3_666 3_666 ? O5 Mn3 O3 84.62(7) 4_575 3_666 ? N6 Mn3 O3 100.39(6) . 3_666 ? O2 Mn3 O8 86.42(6) 3_666 . ? O5 Mn3 O8 104.23(7) 4_575 . ? N6 Mn3 O8 74.24(6) . . ? O3 Mn3 O8 169.85(6) 3_666 . ? O2 Mn3 N4 94.88(6) 3_666 4_575 ? O5 Mn3 N4 74.52(6) 4_575 4_575 ? N6 Mn3 N4 164.15(8) . 4_575 ? O3 Mn3 N4 90.46(7) 3_666 4_575 ? O8 Mn3 N4 96.63(7) . 4_575 ? Mn1 O1W H1A 132.0 . . ? Mn1 O1W H1B 124.5 . . ? H1A O1W H1B 103.4 . . ? C1 O1 Mn2 137.98(14) . . ? C1 O1 Mn1 117.66(14) . . ? Mn2 O1 Mn1 103.21(6) . . ? C1 O2 Mn3 127.75(14) . 3_666 ? Mn1 O2W H2A 126.0 . . ? Mn1 O2W H2B 128.8 . . ? H2A O2W H2B 105.1 . . ? Mn1 O3W H3A 112.3 . . ? Mn1 O3W H3B 114.3 . . ? H3A O3W H3B 104.7 . . ? C4 O3 Mn3 127.49(14) . 3_666 ? Mn2 O4W H4A 120.1 . . ? Mn2 O4W H4B 126.8 . . ? H4A O4W H4B 104.6 . . ? C4 O4 Mn1 140.97(14) . 2_546 ? C4 O4 Mn2 116.32(13) . 2_546 ? Mn1 O4 Mn2 101.30(6) 2_546 2_546 ? C5 O5 Mn3 117.69(14) . 4_576 ? C5 O6 Mn2 120.27(14) . . ? C8 O7 Mn2 133.22(15) . . ? C8 O8 Mn3 118.20(14) . . ? N2 N1 C2 109.31(18) . . ? N2 N1 Mn1 131.89(15) . . ? C2 N1 Mn1 118.71(14) . . ? N1 N2 N3 108.13(19) . . ? N2 N3 C3 109.30(18) . . ? N2 N3 Mn2 131.88(14) . 2_546 ? C3 N3 Mn2 118.40(14) . 2_546 ? N5 N4 C6 108.60(18) . . ? N5 N4 Mn3 138.41(15) . 4_576 ? C6 N4 Mn3 112.58(14) . 4_576 ? N4 N5 N6 108.53(18) . . ? N5 N6 C7 109.18(18) . . ? N5 N6 Mn3 136.29(14) . . ? C7 N6 Mn3 114.18(15) . . ? O2 C1 O1 123.8(2) . . ? O2 C1 C2 121.1(2) . . ? O1 C1 C2 115.15(19) . . ? N1 C2 C3 106.63(18) . . ? N1 C2 C1 116.47(19) . . ? C3 C2 C1 136.56(19) . . ? N3 C3 C2 106.62(18) . . ? N3 C3 C4 117.31(19) . . ? C2 C3 C4 136.07(19) . . ? O3 C4 O4 124.2(2) . . ? O3 C4 C3 120.0(2) . . ? O4 C4 C3 115.74(19) . . ? O6 C5 O5 123.9(2) . . ? O6 C5 C6 120.1(2) . . ? O5 C5 C6 115.9(2) . . ? N4 C6 C7 107.19(19) . . ? N4 C6 C5 117.34(19) . . ? C7 C6 C5 135.4(2) . . ? N6 C7 C6 106.5(2) . . ? N6 C7 C8 116.67(19) . . ? C6 C7 C8 136.5(2) . . ? O7 C8 O8 123.9(2) . . ? O7 C8 C7 120.4(2) . . ? O8 C8 C7 115.69(19) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.397 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.074