# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xiao-Ming Chen' _publ_contact_author_email CXM@MAIL.SYSU.EDU.CN _publ_section_title ; 3D geometrically frustrated magnets assembled by transition metal ion and 1,2,3-triazole-4,5-dicarboxylate as triangular nodes ; loop_ _publ_author_name 'Xiao-Ming Chen.' 'Jian-Bin Lin.' 'Wei Xue.' 'Wei-Xiong Zhang.' ; Yan-Zhen Zheng ; # Attachment '1.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 691173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H9 Co N4 O4.50' _chemical_formula_weight 268.10 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 9.8941(7) _cell_length_b 9.8941(7) _cell_length_c 9.8941(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 968.57(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 1.780 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8283 _exptl_absorpt_correction_T_max 0.8421 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 9834 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 26.00 _reflns_number_total 650 _reflns_number_gt 620 _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^)+(0.0461P)^2^+0.1254P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(5) _refine_ls_number_reflns 650 _refine_ls_number_parameters 97 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.075 _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 Co1 Co -0.63780(4) 0.13780(4) -0.13780(4) 0.0625(2) Uani 1 3 d S . . C1 C -0.4736(12) -0.0995(10) -0.2461(10) 0.089(2) Uani 0.33 1 d PD A -1 C2 C -0.5543(7) -0.1484(6) -0.3656(6) 0.0447(12) Uani 0.33 1 d PD A -1 C3 C -0.6704(7) -0.0981(6) -0.4263(7) 0.0447(12) Uani 0.33 1 d PD A -1 C4 C -0.7581(12) 0.0215(11) -0.3971(11) 0.089(2) Uani 0.33 1 d PD A -1 N1 N -0.5180(7) -0.2607(6) -0.4347(6) 0.0554(10) Uani 0.33 1 d PD . -1 N2 N -0.6070(8) -0.2787(9) -0.5327(10) 0.0554(10) Uani 0.33 1 d PD B -1 N3 N -0.6982(6) -0.1829(6) -0.5293(7) 0.0554(10) Uani 0.33 1 d PD . -1 O1 O -0.4239(14) -0.2157(9) -0.2270(14) 0.096(3) Uani 0.33 1 d PD . -1 O2 O -0.4762(15) -0.0152(11) -0.1501(10) 0.095(3) Uani 0.33 1 d PD A -1 O3 O -0.7736(16) 0.1187(11) -0.3174(10) 0.095(3) Uani 0.33 1 d PD A -1 O4 O -0.8011(13) 0.0298(11) -0.5163(10) 0.096(3) Uani 0.33 1 d PD . -1 N4 N -0.399(4) -0.130(3) 0.105(3) 0.135(9) Uani 0.33 1 d PD C -1 H4A H -0.4106 -0.0921 0.1870 0.162 Uiso 0.33 1 d PR C -1 H4B H -0.4470 -0.0835 0.0441 0.162 Uiso 0.33 1 d PR C -1 C5 C -0.443(3) -0.270(3) 0.110(2) 0.139(6) Uani 0.33 1 d PD C -1 H5A H -0.5387 -0.2546 0.1310 0.209 Uiso 0.33 1 d PR C -1 H5B H -0.4019 -0.3238 0.1824 0.209 Uiso 0.33 1 d PR C -1 H5C H -0.4358 -0.3193 0.0243 0.209 Uiso 0.33 1 d PR C -1 C6 C -0.256(4) -0.130(3) 0.069(3) 0.139(6) Uani 0.33 1 d PD C -1 H6A H -0.2144 -0.0414 0.0579 0.209 Uiso 0.33 1 d PR C -1 H6B H -0.2493 -0.1811 -0.0157 0.209 Uiso 0.33 1 d PR C -1 H6C H -0.2097 -0.1801 0.1411 0.209 Uiso 0.33 1 d PR C -1 O1W O -0.326(2) -0.029(4) 0.367(2) 0.162(11) Uani 0.17 1 d P . . H1WA H -0.3099 -0.0958 0.4195 0.244 Uiso 0.17 1 d PR . . H1WB H -0.2562 0.0207 0.3627 0.244 Uiso 0.17 1 d PR . . 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 Co1 0.0625(2) 0.0625(2) 0.0625(2) -0.01081(18) 0.01081(18) -0.01081(18) C1 0.063(6) 0.119(8) 0.086(7) 0.007(6) -0.022(5) 0.038(5) C2 0.046(3) 0.046(3) 0.042(3) 0.002(2) 0.005(2) -0.004(2) C3 0.046(3) 0.046(3) 0.042(3) 0.002(2) 0.005(2) -0.004(2) C4 0.063(6) 0.119(8) 0.086(7) 0.007(6) -0.022(5) 0.038(5) N1 0.057(2) 0.048(2) 0.061(3) -0.0005(17) -0.0097(19) 0.0093(18) N2 0.057(2) 0.048(2) 0.061(3) -0.0005(17) -0.0097(19) 0.0093(18) N3 0.057(2) 0.048(2) 0.061(3) -0.0005(17) -0.0097(19) 0.0093(18) O1 0.124(7) 0.065(3) 0.098(5) -0.029(3) -0.028(5) 0.015(4) O2 0.130(6) 0.085(4) 0.069(4) -0.016(4) -0.033(4) 0.038(4) O3 0.130(6) 0.085(4) 0.069(4) -0.016(4) -0.033(4) 0.038(4) O4 0.124(7) 0.065(3) 0.098(5) -0.029(3) -0.028(5) 0.015(4) N4 0.109(14) 0.14(2) 0.158(19) -0.038(13) -0.064(13) 0.074(13) C5 0.19(2) 0.129(11) 0.102(10) -0.009(9) -0.045(9) -0.007(14) C6 0.19(2) 0.129(11) 0.102(10) -0.009(9) -0.045(9) -0.007(14) O1W 0.080(10) 0.32(3) 0.087(12) -0.01(2) -0.004(10) 0.027(16) _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 Co1 N1 1.975(6) 3_454 ? Co1 N1 1.975(6) 8_454 ? Co1 N1 1.975(6) 10_454 ? Co1 N3 1.996(6) 11_444 ? Co1 N3 1.996(6) 5_565 ? Co1 N3 1.996(6) 2_355 ? Co1 O1 2.065(10) 3_454 ? Co1 O1 2.065(10) 8_454 ? Co1 O1 2.065(10) 10_454 ? Co1 O4 2.135(9) 5_565 ? Co1 O4 2.135(9) 11_444 ? Co1 O4 2.135(9) 2_355 ? C1 O2 1.264(9) . ? C1 O1 1.265(9) . ? C1 C2 1.506(9) . ? C2 N1 1.353(8) . ? C2 C3 1.389(7) . ? C3 N3 1.348(8) . ? C3 C4 1.496(9) . ? C4 O3 1.254(9) . ? C4 O4 1.256(9) . ? N1 N2 1.322(8) . ? N1 Co1 1.975(6) 3_444 ? N2 N3 1.309(8) . ? N3 Co1 1.996(6) 2_354 ? O1 Co1 2.065(10) 3_444 ? O4 Co1 2.135(9) 2_354 ? N4 C5 1.453(10) . ? N4 C6 1.453(10) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C5 O1W 1.18(4) 12_455 ? C5 H5A 0.9800 . ? C5 H5B 0.9799 . ? C5 H5C 0.9801 . ? C6 O1W 1.36(4) 6_445 ? C6 H6A 0.9800 . ? C6 H6B 0.9801 . ? C6 H6C 0.9799 . ? O1W C5 1.18(4) 6_445 ? O1W C6 1.36(4) 12_455 ? O1W H1WA 0.8499 . ? O1W H1WB 0.8499 . ? 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 N1 Co1 N1 107.36(18) 3_454 8_454 ? N1 Co1 N1 107.36(18) 3_454 10_454 ? N1 Co1 N1 107.36(18) 8_454 10_454 ? N1 Co1 N3 138.0(3) 3_454 11_444 ? N1 Co1 N3 41.2(2) 8_454 11_444 ? N1 Co1 N3 109.0(3) 10_454 11_444 ? N1 Co1 N3 41.2(2) 3_454 5_565 ? N1 Co1 N3 109.0(3) 8_454 5_565 ? N1 Co1 N3 138.0(3) 10_454 5_565 ? N3 Co1 N3 112.07(17) 11_444 5_565 ? N1 Co1 N3 109.0(3) 3_454 2_355 ? N1 Co1 N3 138.0(3) 8_454 2_355 ? N1 Co1 N3 41.2(2) 10_454 2_355 ? N3 Co1 N3 112.07(17) 11_444 2_355 ? N3 Co1 N3 112.07(17) 5_565 2_355 ? N1 Co1 O1 69.4(4) 3_454 3_454 ? N1 Co1 O1 96.4(4) 8_454 3_454 ? N1 Co1 O1 155.7(4) 10_454 3_454 ? N3 Co1 O1 85.2(4) 11_444 3_454 ? N3 Co1 O1 29.0(3) 5_565 3_454 ? N3 Co1 O1 115.6(5) 2_355 3_454 ? N1 Co1 O1 155.7(4) 3_454 8_454 ? N1 Co1 O1 69.4(4) 8_454 8_454 ? N1 Co1 O1 96.4(4) 10_454 8_454 ? N3 Co1 O1 29.0(3) 11_444 8_454 ? N3 Co1 O1 115.6(5) 5_565 8_454 ? N3 Co1 O1 85.2(4) 2_355 8_454 ? O1 Co1 O1 86.8(5) 3_454 8_454 ? N1 Co1 O1 96.4(4) 3_454 10_454 ? N1 Co1 O1 155.7(4) 8_454 10_454 ? N1 Co1 O1 69.4(4) 10_454 10_454 ? N3 Co1 O1 115.6(5) 11_444 10_454 ? N3 Co1 O1 85.2(4) 5_565 10_454 ? N3 Co1 O1 29.0(3) 2_355 10_454 ? O1 Co1 O1 86.8(5) 3_454 10_454 ? O1 Co1 O1 86.8(5) 8_454 10_454 ? N1 Co1 O4 30.1(3) 3_454 5_565 ? N1 Co1 O4 114.3(4) 8_454 5_565 ? N1 Co1 O4 77.5(4) 10_454 5_565 ? N3 Co1 O4 155.4(4) 11_444 5_565 ? N3 Co1 O4 68.9(4) 5_565 5_565 ? N3 Co1 O4 88.7(4) 2_355 5_565 ? O1 Co1 O4 97.9(5) 3_454 5_565 ? O1 Co1 O4 173.5(6) 8_454 5_565 ? O1 Co1 O4 89.0(6) 10_454 5_565 ? N1 Co1 O4 77.5(4) 3_454 11_444 ? N1 Co1 O4 30.1(3) 8_454 11_444 ? N1 Co1 O4 114.3(4) 10_454 11_444 ? N3 Co1 O4 68.9(4) 11_444 11_444 ? N3 Co1 O4 88.7(4) 5_565 11_444 ? N3 Co1 O4 155.4(4) 2_355 11_444 ? O1 Co1 O4 89.0(6) 3_454 11_444 ? O1 Co1 O4 97.9(5) 8_454 11_444 ? O1 Co1 O4 173.5(6) 10_454 11_444 ? O4 Co1 O4 86.7(5) 5_565 11_444 ? N1 Co1 O4 114.3(4) 3_454 2_355 ? N1 Co1 O4 77.5(4) 8_454 2_355 ? N1 Co1 O4 30.1(3) 10_454 2_355 ? N3 Co1 O4 88.7(4) 11_444 2_355 ? N3 Co1 O4 155.4(4) 5_565 2_355 ? N3 Co1 O4 68.9(4) 2_355 2_355 ? O1 Co1 O4 173.5(6) 3_454 2_355 ? O1 Co1 O4 89.0(6) 8_454 2_355 ? O1 Co1 O4 97.9(5) 10_454 2_355 ? O4 Co1 O4 86.7(5) 5_565 2_355 ? O4 Co1 O4 86.7(5) 11_444 2_355 ? O2 C1 O1 119.7(10) . . ? O2 C1 C2 142.3(11) . . ? O1 C1 C2 91.8(9) . . ? N1 C2 C3 107.2(5) . . ? N1 C2 C1 121.3(8) . . ? C3 C2 C1 131.5(8) . . ? N3 C3 C2 105.8(5) . . ? N3 C3 C4 121.3(8) . . ? C2 C3 C4 132.9(9) . . ? O3 C4 O4 120.0(9) . . ? O3 C4 C3 143.1(11) . . ? O4 C4 C3 93.9(9) . . ? N2 N1 C2 107.7(6) . . ? N2 N1 Co1 135.9(5) . 3_444 ? C2 N1 Co1 116.2(5) . 3_444 ? N3 N2 N1 110.0(7) . . ? N2 N3 C3 109.2(6) . . ? N2 N3 Co1 135.1(6) . 2_354 ? C3 N3 Co1 115.7(5) . 2_354 ? C1 O1 Co1 131.0(11) . 3_444 ? C1 O2 Co1 120.6(9) . . ? C4 O3 Co1 119.5(8) . . ? C4 O4 Co1 125.0(10) . 2_354 ? C5 N4 C6 107.5(10) . . ? C5 N4 H4A 109.4 . . ? C6 N4 H4A 110.4 . . ? C5 N4 H4B 110.5 . . ? C6 N4 H4B 110.5 . . ? H4A N4 H4B 108.5 . . ? O1W C5 N4 149(2) 12_455 . ? O1W C5 H5A 78.1 12_455 . ? N4 C5 H5A 98.5 . . ? O1W C5 H5B 42.6 12_455 . ? N4 C5 H5B 114.4 . . ? H5A C5 H5B 109.5 . . ? O1W C5 H5C 94.6 12_455 . ? N4 C5 H5C 114.9 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O1W C6 N4 161(2) 6_445 . ? O1W C6 H6A 82.7 6_445 . ? N4 C6 H6A 115.9 . . ? O1W C6 H6B 61.7 6_445 . ? N4 C6 H6B 106.2 . . ? H6A C6 H6B 109.5 . . ? O1W C6 H6C 68.1 6_445 . ? N4 C6 H6C 106.1 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 O1W C6 14(2) 6_445 12_455 ? C5 O1W H1WA 114.6 6_445 . ? C6 O1W H1WA 112.5 12_455 . ? C5 O1W H1WB 121.7 6_445 . ? C6 O1W H1WB 112.3 12_455 . ? H1WA O1W H1WB 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.240 _refine_diff_density_min -0.146 _refine_diff_density_rms 0.047 # Attachment '2.cif' data_d _database_code_depnum_ccdc_archive 'CCDC 691174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Mn N4 O4.50' _chemical_formula_weight 263.10 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 Cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 10.2304(4) _cell_length_b 10.2304(4) _cell_length_c 10.2304(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1070.72(7) _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 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 1.240 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8757 _exptl_absorpt_correction_T_max 0.8861 _exptl_absorpt_process_details ? _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 ? _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 9249 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0134 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 24.82 _reflns_number_total 627 _reflns_number_gt 596 _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^)+(0.1401P)^2^+1.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(2) _refine_ls_number_reflns 627 _refine_ls_number_parameters 82 _refine_ls_number_restraints 113 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.2546 _refine_ls_wR_factor_gt 0.2513 _refine_ls_goodness_of_fit_ref 1.208 _refine_ls_restrained_S_all 1.146 _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 -0.37401(19) -0.12599(19) -0.87401(19) 0.0973(11) Uani 1 3 d SU . . C1 C -0.520(3) 0.136(3) -0.763(2) 0.100(7) Uani 0.33 1 d PDU A -1 C2 C -0.4396(13) 0.1695(16) -0.6470(14) 0.067(5) Uani 0.33 1 d PDU A -1 C3 C -0.3298(14) 0.1097(14) -0.5980(17) 0.067(5) Uani 0.33 1 d PDU A -1 C4 C -0.232(2) 0.003(2) -0.610(2) 0.100(7) Uani 0.33 1 d PDU A -1 N1 N -0.4649(17) 0.2715(15) -0.5671(16) 0.089(4) Uani 0.33 1 d PDU . -1 N2 N -0.375(2) 0.274(2) -0.4743(17) 0.089(4) Uani 0.33 1 d PDU B -1 N3 N -0.2921(18) 0.177(2) -0.4908(16) 0.089(4) Uani 0.33 1 d PDU . -1 O1 O -0.610(3) 0.219(3) -0.772(4) 0.181(12) Uani 0.33 1 d PDU . -1 O2 O -0.507(3) 0.048(3) -0.849(3) 0.131(7) Uani 0.33 1 d PDU A -1 O3 O -0.223(3) -0.077(3) -0.701(3) 0.131(7) Uani 0.33 1 d PDU A -1 O4 O -0.210(4) -0.020(4) -0.493(3) 0.181(12) Uani 0.33 1 d PDU . -1 N4 N -0.367(2) 0.367(2) -1.133(2) 0.28(2) Uani 1 3 d SDU . . H4A H -0.3158 0.3158 -1.1842 0.333 Uiso 1 3 calc SR . . C5 C -0.484(3) 0.298(2) -1.097(6) 0.34(3) Uani 0.67 1 d PDU . . H5A H -0.5493 0.3104 -1.1634 0.505 Uiso 0.67 1 calc PR . . H5B H -0.5159 0.3304 -1.0151 0.505 Uiso 0.67 1 calc PR . . H5C H -0.4648 0.2063 -1.0891 0.505 Uiso 0.67 1 calc PR . . O1W O -0.601(2) 0.101(2) -1.101(2) 0.197(19) Uani 0.50 3 d SPU . . H1WA H -0.6638 0.1070 -1.0490 0.296 Uiso 0.17 1 d PR . . H1WB H -0.6320 0.0979 -1.1805 0.296 Uiso 0.17 1 d PR . . 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 0.0973(11) 0.0973(11) 0.0973(11) -0.0266(9) 0.0266(9) -0.0266(9) C1 0.063(11) 0.106(14) 0.129(17) -0.042(14) -0.034(9) 0.050(10) C2 0.051(6) 0.064(7) 0.085(13) -0.015(8) 0.013(8) 0.019(7) C3 0.051(6) 0.064(7) 0.085(13) -0.015(8) 0.013(8) 0.019(7) C4 0.063(11) 0.106(14) 0.129(17) -0.042(14) -0.034(9) 0.050(10) N1 0.088(8) 0.126(12) 0.053(6) 0.021(7) -0.022(6) -0.005(8) N2 0.088(8) 0.126(12) 0.053(6) 0.021(7) -0.022(6) -0.005(8) N3 0.088(8) 0.126(12) 0.053(6) 0.021(7) -0.022(6) -0.005(8) O1 0.19(2) 0.120(15) 0.23(2) 0.043(16) 0.00(2) -0.021(16) O2 0.115(11) 0.137(13) 0.142(14) -0.081(11) -0.035(10) 0.068(10) O3 0.115(11) 0.137(13) 0.142(14) -0.081(11) -0.035(10) 0.068(10) O4 0.19(2) 0.120(15) 0.23(2) 0.043(16) 0.00(2) -0.021(16) N4 0.28(2) 0.28(2) 0.28(2) -0.011(19) 0.011(19) 0.011(19) C5 0.45(6) 0.061(10) 0.50(7) 0.02(2) 0.23(5) 0.02(2) O1W 0.197(19) 0.197(19) 0.197(19) 0.046(16) -0.046(16) 0.046(16) _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 N1 2.045(14) 10_553 ? Mn1 N1 2.045(14) 3_443 ? Mn1 N1 2.045(14) 8_454 ? Mn1 O4 2.11(3) 5_554 ? Mn1 O4 2.11(3) 2_454 ? Mn1 O4 2.11(3) 11_444 ? Mn1 N3 2.141(13) 2_454 ? Mn1 N3 2.141(13) 11_444 ? Mn1 N3 2.141(13) 5_554 ? Mn1 O1 2.19(3) 10_553 ? Mn1 O1 2.19(3) 8_454 ? Mn1 O1 2.19(3) 3_443 ? C1 O1 1.255(10) . ? C1 O2 1.257(10) . ? C1 C2 1.490(9) . ? C2 N1 1.350(9) . ? C2 C3 1.374(9) . ? C3 N3 1.350(9) . ? C3 C4 1.485(9) . ? C4 O4 1.245(10) . ? C4 O3 1.246(10) . ? N1 N2 1.319(9) . ? N1 Mn1 2.045(14) 3_453 ? N2 N3 1.319(9) . ? N3 Mn1 2.141(13) 2_455 ? O1 Mn1 2.19(3) 3_453 ? O4 Mn1 2.11(3) 2_455 ? N4 C5 1.437(10) 10_563 ? N4 C5 1.437(10) . ? N4 C5 1.437(10) 7_353 ? N4 H4A 0.9100 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? O1W H1WA 0.8359 . ? O1W H1WB 0.8710 . ? 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 N1 Mn1 N1 109.1(5) 10_553 3_443 ? N1 Mn1 N1 109.1(5) 10_553 8_454 ? N1 Mn1 N1 109.1(5) 3_443 8_454 ? N1 Mn1 O4 81.0(11) 10_553 5_554 ? N1 Mn1 O4 28.1(10) 3_443 5_554 ? N1 Mn1 O4 121.6(11) 8_454 5_554 ? N1 Mn1 O4 28.1(10) 10_553 2_454 ? N1 Mn1 O4 121.6(11) 3_443 2_454 ? N1 Mn1 O4 81.0(11) 8_454 2_454 ? O4 Mn1 O4 96.7(16) 5_554 2_454 ? N1 Mn1 O4 121.6(11) 10_553 11_444 ? N1 Mn1 O4 81.0(11) 3_443 11_444 ? N1 Mn1 O4 28.1(10) 8_454 11_444 ? O4 Mn1 O4 96.7(16) 5_554 11_444 ? O4 Mn1 O4 96.7(16) 2_454 11_444 ? N1 Mn1 N3 38.2(6) 10_553 2_454 ? N1 Mn1 N3 110.6(6) 3_443 2_454 ? N1 Mn1 N3 135.7(6) 8_454 2_454 ? O4 Mn1 N3 87.8(10) 5_554 2_454 ? O4 Mn1 N3 61.7(13) 2_454 2_454 ? O4 Mn1 N3 158.4(11) 11_444 2_454 ? N1 Mn1 N3 110.6(6) 10_553 11_444 ? N1 Mn1 N3 135.7(6) 3_443 11_444 ? N1 Mn1 N3 38.2(6) 8_454 11_444 ? O4 Mn1 N3 158.4(11) 5_554 11_444 ? O4 Mn1 N3 87.8(10) 2_454 11_444 ? O4 Mn1 N3 61.7(13) 11_444 11_444 ? N3 Mn1 N3 112.7(5) 2_454 11_444 ? N1 Mn1 N3 135.7(6) 10_553 5_554 ? N1 Mn1 N3 38.2(6) 3_443 5_554 ? N1 Mn1 N3 110.6(6) 8_454 5_554 ? O4 Mn1 N3 61.7(13) 5_554 5_554 ? O4 Mn1 N3 158.4(11) 2_454 5_554 ? O4 Mn1 N3 87.8(10) 11_444 5_554 ? N3 Mn1 N3 112.7(5) 2_454 5_554 ? N3 Mn1 N3 112.7(5) 11_444 5_554 ? N1 Mn1 O1 76.7(8) 10_553 10_553 ? N1 Mn1 O1 102.3(12) 3_443 10_553 ? N1 Mn1 O1 143.4(12) 8_454 10_553 ? O4 Mn1 O1 94.9(16) 5_554 10_553 ? O4 Mn1 O1 98.4(15) 2_454 10_553 ? O4 Mn1 O1 159.6(13) 11_444 10_553 ? N3 Mn1 O1 38.5(9) 2_454 10_553 ? N3 Mn1 O1 105.3(12) 11_444 10_553 ? N3 Mn1 O1 83.1(11) 5_554 10_553 ? N1 Mn1 O1 102.3(12) 10_553 8_454 ? N1 Mn1 O1 143.4(12) 3_443 8_454 ? N1 Mn1 O1 76.7(8) 8_454 8_454 ? O4 Mn1 O1 159.6(13) 5_554 8_454 ? O4 Mn1 O1 94.9(16) 2_454 8_454 ? O4 Mn1 O1 98.4(15) 11_444 8_454 ? N3 Mn1 O1 83.1(11) 2_454 8_454 ? N3 Mn1 O1 38.5(9) 11_444 8_454 ? N3 Mn1 O1 105.3(12) 5_554 8_454 ? O1 Mn1 O1 66.8(14) 10_553 8_454 ? N1 Mn1 O1 143.4(12) 10_553 3_443 ? N1 Mn1 O1 76.7(8) 3_443 3_443 ? N1 Mn1 O1 102.3(11) 8_454 3_443 ? O4 Mn1 O1 98.4(15) 5_554 3_443 ? O4 Mn1 O1 159.6(13) 2_454 3_443 ? O4 Mn1 O1 94.9(16) 11_444 3_443 ? N3 Mn1 O1 105.3(12) 2_454 3_443 ? N3 Mn1 O1 83.1(11) 11_444 3_443 ? N3 Mn1 O1 38.5(9) 5_554 3_443 ? O1 Mn1 O1 66.8(14) 10_553 3_443 ? O1 Mn1 O1 66.8(14) 8_454 3_443 ? O1 C1 O2 120.6(18) . . ? O1 C1 C2 108(2) . . ? O2 C1 C2 131(2) . . ? N1 C2 C3 106.2(9) . . ? N1 C2 C1 123.9(16) . . ? C3 C2 C1 129.9(18) . . ? N3 C3 C2 107.7(9) . . ? N3 C3 C4 104.4(18) . . ? C2 C3 C4 147.9(19) . . ? O4 C4 O3 126(2) . . ? O4 C4 C3 100(2) . . ? O3 C4 C3 127(2) . . ? N2 N1 C2 108.5(9) . . ? N2 N1 Mn1 139.7(13) . 3_453 ? C2 N1 Mn1 111.9(11) . 3_453 ? N3 N2 N1 110.0(10) . . ? N2 N3 C3 107.6(9) . . ? N2 N3 Mn1 128.6(13) . 2_455 ? C3 N3 Mn1 123.8(14) . 2_455 ? C1 O1 Mn1 120(3) . 3_453 ? C1 O2 Mn1 135.0(18) . . ? C4 O3 Mn1 129.7(17) . . ? C4 O4 Mn1 120(2) . 2_455 ? C5 N4 C5 109(2) 10_563 . ? C5 N4 C5 109(2) 10_563 7_353 ? C5 N4 C5 109(2) . 7_353 ? C5 N4 H4A 110.0 10_563 . ? C5 N4 H4A 110.0 . . ? C5 N4 H4A 110.0 7_353 . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? H1WA O1W H1WB 108.8 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.82 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.321 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.091 # Attachment '3.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 691175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H9.20 Mn N4 O6.60' _chemical_formula_weight 273.89 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 Hexagonal _symmetry_space_group_name_H-M P6(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' '-x, -y, z+1/2' 'y, -x+y, z+5/6' 'x-y, x, z+1/6' _cell_length_a 14.3295(6) _cell_length_b 14.3295(6) _cell_length_c 10.0523(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1787.55(18) _cell_formula_units_Z 6 _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 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8400 _exptl_absorpt_correction_T_max 0.9251 _exptl_absorpt_process_details ? _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 ? _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 12457 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.04 _reflns_number_total 2349 _reflns_number_gt 2278 _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^)+(0.0968P)^2^+0.5141P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 2349 _refine_ls_number_parameters 133 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1314 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.87483(4) 0.33960(4) 0.06239(6) 0.0283(2) Uani 1 1 d . . . C1 C 0.6813(4) 0.2203(3) -0.1351(4) 0.0361(9) Uani 1 1 d . . . C2 C 0.6094(3) 0.1285(3) -0.0480(4) 0.0269(7) Uani 1 1 d . . . C3 C 0.6234(3) 0.0793(3) 0.0626(4) 0.0271(7) Uani 1 1 d . . . C4 C 0.7142(3) 0.0973(3) 0.1525(4) 0.0336(8) Uani 1 1 d . . . N1 N 0.5050(2) 0.0703(2) -0.0833(4) 0.0318(7) Uani 1 1 d . . . N2 N 0.4563(3) -0.0118(3) 0.0005(4) 0.0348(8) Uani 1 1 d . . . N3 N 0.5263(2) -0.0083(2) 0.0889(3) 0.0299(7) Uani 1 1 d . . . O1 O 0.6362(3) 0.2399(3) -0.2302(4) 0.0532(9) Uani 1 1 d . . . O2 O 0.7815(2) 0.2716(3) -0.1149(3) 0.0469(8) Uani 1 1 d . . . O3 O 0.7975(3) 0.1875(3) 0.1578(4) 0.0616(11) Uani 1 1 d . . . O4 O 0.6970(2) 0.0185(2) 0.2235(4) 0.0432(7) Uani 1 1 d . . . N4 N 0.2822(5) -0.2344(4) -0.0647(7) 0.0804(17) Uani 1 1 d . . . H4A H 0.2419 -0.2516 -0.1390 0.121 Uiso 1 1 d R . . H4B H 0.3311 -0.1637 -0.0696 0.121 Uiso 1 1 d R . . H4C H 0.3168 -0.2709 -0.0825 0.121 Uiso 1 1 d R . . H4D H 0.2376 -0.2676 0.0041 0.121 Uiso 1 1 d R . . O1W O 0.1238(9) -0.3176(9) 0.1214(14) 0.174(5) Uiso 1 1 d . . . H1WA H 0.1516 -0.3089 0.1984 0.261 Uiso 1 1 d R . . H1WB H 0.0702 -0.3110 0.0994 0.261 Uiso 1 1 d R . . O2W O -0.038(2) -0.286(2) 0.059(3) 0.261(8) Uiso 0.60 1 d P . . H2WA H -0.0515 -0.2530 0.1199 0.392 Uiso 0.60 1 d PR . . H2WB H -0.0364 -0.2481 -0.0074 0.392 Uiso 0.60 1 d PR . . O3W O -0.091(3) -0.173(3) 0.241(4) 0.261(8) Uiso 0.50 1 d P . . H3WA H -0.0369 -0.1405 0.2923 0.392 Uiso 0.50 1 d PR . . H3WB H -0.1570 -0.2057 0.2652 0.392 Uiso 0.50 1 d PR . . O4W O -0.029(3) -0.191(2) -0.227(4) 0.261(8) Uiso 0.50 1 d P . . H4WA H -0.0294 -0.2344 -0.2848 0.392 Uiso 0.50 1 d PR . . H4WB H -0.0785 -0.1857 -0.2661 0.392 Uiso 0.50 1 d PR . . 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 0.0213(3) 0.0290(3) 0.0270(3) 0.0000(2) 0.0020(2) 0.0070(2) C1 0.041(2) 0.0235(18) 0.027(2) 0.0000(15) -0.0031(15) 0.0041(16) C2 0.0263(16) 0.0220(16) 0.0247(16) 0.0003(14) 0.0009(13) 0.0064(14) C3 0.0273(16) 0.0212(15) 0.0303(18) 0.0004(15) 0.0004(15) 0.0103(13) C4 0.0295(18) 0.0315(18) 0.033(2) 0.0009(16) -0.0040(15) 0.0097(15) N1 0.0317(15) 0.0265(15) 0.0338(18) 0.0039(13) 0.0015(13) 0.0122(13) N2 0.0300(15) 0.0280(15) 0.0422(19) 0.0123(15) 0.0025(14) 0.0113(13) N3 0.0265(14) 0.0253(14) 0.0348(18) 0.0052(13) 0.0020(13) 0.0107(12) O1 0.0448(18) 0.0403(17) 0.0429(18) 0.0154(14) -0.0094(14) -0.0024(14) O2 0.0327(14) 0.0465(17) 0.0300(15) 0.0027(14) 0.0001(12) -0.0038(13) O3 0.0446(19) 0.0438(17) 0.056(2) 0.0217(16) -0.0159(17) -0.0080(15) O4 0.0365(14) 0.0351(14) 0.0491(18) 0.0135(14) -0.0077(14) 0.0112(12) N4 0.079(4) 0.061(3) 0.089(4) -0.004(3) -0.029(3) 0.027(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 Mn1 O3 2.118(3) . ? Mn1 O2 2.147(3) . ? Mn1 O4 2.201(3) 5_664 ? Mn1 O1 2.206(3) 2_655 ? Mn1 N1 2.227(3) 2_655 ? Mn1 N3 2.240(3) 5_664 ? C1 O2 1.261(5) . ? C1 O1 1.262(6) . ? C1 C2 1.484(5) . ? C2 N1 1.347(5) . ? C2 C3 1.383(6) . ? C3 N3 1.355(4) . ? C3 C4 1.497(5) . ? C4 O3 1.248(5) . ? C4 O4 1.252(5) . ? N1 N2 1.326(5) . ? N1 Mn1 2.227(3) 3_664 ? N2 N3 1.322(5) . ? N3 Mn1 2.240(3) 6_545 ? O1 Mn1 2.206(3) 3_664 ? O4 Mn1 2.201(3) 6_545 ? N4 H4A 0.8999 . ? N4 H4B 0.9000 . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8499 . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8499 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8498 . ? O4W H4WB 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 O3 Mn1 O2 91.30(14) . . ? O3 Mn1 O4 85.90(15) . 5_664 ? O2 Mn1 O4 109.42(14) . 5_664 ? O3 Mn1 O1 101.12(17) . 2_655 ? O2 Mn1 O1 84.91(13) . 2_655 ? O4 Mn1 O1 164.06(13) 5_664 2_655 ? O3 Mn1 N1 95.10(15) . 2_655 ? O2 Mn1 N1 158.38(13) . 2_655 ? O4 Mn1 N1 91.65(13) 5_664 2_655 ? O1 Mn1 N1 73.60(12) 2_655 2_655 ? O3 Mn1 N3 155.35(16) . 5_664 ? O2 Mn1 N3 83.58(11) . 5_664 ? O4 Mn1 N3 73.27(11) 5_664 5_664 ? O1 Mn1 N3 102.41(14) 2_655 5_664 ? N1 Mn1 N3 98.47(12) 2_655 5_664 ? O2 C1 O1 123.5(4) . . ? O2 C1 C2 120.4(4) . . ? O1 C1 C2 116.1(4) . . ? N1 C2 C3 107.1(3) . . ? N1 C2 C1 117.2(3) . . ? C3 C2 C1 135.5(3) . . ? N3 C3 C2 106.7(3) . . ? N3 C3 C4 116.3(3) . . ? C2 C3 C4 137.1(3) . . ? O3 C4 O4 124.3(4) . . ? O3 C4 C3 120.2(4) . . ? O4 C4 C3 115.3(3) . . ? N2 N1 C2 108.1(3) . . ? N2 N1 Mn1 137.4(3) . 3_664 ? C2 N1 Mn1 114.1(2) . 3_664 ? N3 N2 N1 109.9(3) . . ? N2 N3 C3 108.2(3) . . ? N2 N3 Mn1 136.1(2) . 6_545 ? C3 N3 Mn1 113.6(2) . 6_545 ? C1 O1 Mn1 118.5(3) . 3_664 ? C1 O2 Mn1 131.9(3) . . ? C4 O3 Mn1 141.6(3) . . ? C4 O4 Mn1 119.9(2) . 6_545 ? H4A N4 H4B 107.2 . . ? H4A N4 H4C 98.1 . . ? H4B N4 H4C 107.3 . . ? H4A N4 H4D 107.6 . . ? H4B N4 H4D 125.8 . . ? H4C N4 H4D 107.3 . . ? H1WA O1W H1WB 127.2 . . ? H2WA O2W H2WB 99.1 . . ? H3WA O3W H3WB 126.5 . . ? H4WA O4W H4WB 92.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.723 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.125