# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_b _database_code_depnum_ccdc_archive 'CCDC 903326' #TrackingRef 'web_deposit_cif_file_0_SlaviSevov_1348603138.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co-mellitate-MeOH _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H48 Co3 O34' _chemical_formula_weight 937.31 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' 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.5326(14) _cell_length_b 13.1450(14) _cell_length_c 14.9863(16) _cell_angle_alpha 90.00 _cell_angle_beta 122.453(3) _cell_angle_gamma 90.00 _cell_volume 3080.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6193 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.30 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 1.730 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_process_details 'Blessing, R.H. (1995) Acta Cryst. A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16911 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.35 _reflns_number_total 3118 _reflns_number_gt 2750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL-V5.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0345P)^2^+4.1453P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3118 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.342472(16) 0.367821(19) 0.34745(2) 0.00965(9) Uani 1 1 d . . . Co2 Co 0.0000 0.5000 0.0000 0.00947(10) Uani 1 2 d S . . O1 O 0.22315(8) 0.36243(10) 0.33333(11) 0.0106(3) Uani 1 1 d . B . O1S O 0.2682(2) 0.6433(3) 0.4239(3) 0.0306(8) Uani 0.50 1 d P A 2 O2 O 0.15672(9) 0.28811(11) 0.17396(11) 0.0141(3) Uani 1 1 d . B . O3 O 0.46454(10) 0.37858(12) 0.37136(13) 0.0165(3) Uani 1 1 d . B . H3A H 0.4740(17) 0.431(2) 0.364(2) 0.025 Uiso 1 1 d . . . H3B H 0.4753(17) 0.340(2) 0.339(2) 0.025 Uiso 1 1 d . . . O4 O 0.39773(9) 0.30582(11) 0.49737(11) 0.0129(3) Uani 1 1 d . B . H4A H 0.4326(16) 0.3444(19) 0.551(2) 0.019 Uiso 1 1 d . . . H4B H 0.3696(17) 0.276(2) 0.507(2) 0.019 Uiso 1 1 d . . . O5 O 0.32415(10) 0.21727(12) 0.29254(13) 0.0193(3) Uani 1 1 d . B . H5A H 0.3503(18) 0.167(2) 0.300(2) 0.029 Uiso 1 1 d . . . H5B H 0.2779(19) 0.209(2) 0.244(2) 0.029 Uiso 1 1 d . . . O6 O 0.28924(10) 0.42965(12) 0.19841(12) 0.0174(3) Uani 1 1 d . B . H6A H 0.2426(19) 0.427(2) 0.160(2) 0.026 Uiso 1 1 d . . . H6B H 0.3069(18) 0.482(2) 0.194(2) 0.026 Uiso 1 1 d . . . O7 O -0.11214(9) 0.50690(12) -0.00006(12) 0.0131(3) Uani 1 1 d . . . H7A H -0.1058(16) 0.533(2) 0.050(2) 0.020 Uiso 1 1 d . . . H7B H -0.1381(17) 0.457(2) -0.009(2) 0.020 Uiso 1 1 d . . . O8 O 0.00940(10) 0.34419(11) 0.00603(12) 0.0143(3) Uani 1 1 d . . . H8A H 0.0564(18) 0.3198(19) 0.059(2) 0.022 Uiso 1 1 d . . . H8B H -0.0259(17) 0.306(2) -0.004(2) 0.022 Uiso 1 1 d . . . O9 O 0.08513(8) 0.53377(10) 0.16969(10) 0.0112(3) Uani 1 1 d . . . O10 O 0.10063(9) 0.57910(10) 0.32288(11) 0.0117(3) Uani 1 1 d . . . O11 O 0.02326(9) 0.08339(10) 0.15888(11) 0.0137(3) Uani 1 1 d . . . O12 O 0.14819(9) 0.11153(10) 0.31085(11) 0.0146(3) Uani 1 1 d . . . O13 O 0.29710(9) 0.84454(11) -0.00319(12) 0.0127(3) Uani 1 1 d . . . H13A H 0.2896(16) 0.8518(18) 0.048(2) 0.019 Uiso 1 1 d . . . H13B H 0.2526(17) 0.8459(19) -0.055(2) 0.019 Uiso 1 1 d . . . O14 O 0.5000 0.25508(17) 0.2500 0.0205(5) Uani 1 2 d S . . H14B H 0.5415(16) 0.217(2) 0.279(2) 0.031 Uiso 1 1 d . . . O15 O 0.3792(8) 0.5131(11) 0.4198(14) 0.0060(14) Uani 0.50 1 d P B 1 O15A O 0.3606(9) 0.5134(14) 0.4150(17) 0.019(3) Uani 0.50 1 d P B 2 H15A H 0.399(2) 0.541(3) 0.413(3) 0.029 Uiso 1 1 d . C 2 C1 C 0.07753(12) 0.51827(14) 0.24728(15) 0.0091(4) Uani 1 1 d . B . C1S C 0.2961(3) 0.7218(4) 0.5023(4) 0.0321(12) Uani 0.50 1 d P . 2 C2 C 0.15781(12) 0.32560(14) 0.25134(15) 0.0093(4) Uani 1 1 d . . . C3 C 0.07349(12) 0.13502(14) 0.24039(15) 0.0101(4) Uani 1 1 d . B . C4 C 0.03739(12) 0.41878(14) 0.24963(14) 0.0080(4) Uani 1 1 d . . . C5 C 0.07559(12) 0.32689(14) 0.24975(14) 0.0085(4) Uani 1 1 d . B . C6 C 0.03751(11) 0.23514(14) 0.24929(14) 0.0089(4) Uani 1 1 d . . . C7 C 0.3314(3) 0.5655(4) 0.4647(5) 0.0261(12) Uani 0.50 1 d P B 1 H14A H 0.797(2) 0.075(3) 0.446(3) 0.039 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.00876(14) 0.00967(14) 0.01061(15) 0.00075(10) 0.00526(12) -0.00005(10) Co2 0.00956(19) 0.00975(19) 0.00926(19) -0.00039(14) 0.00516(16) -0.00150(14) O1 0.0082(7) 0.0123(7) 0.0108(7) -0.0010(5) 0.0047(6) -0.0010(5) O1S 0.0234(18) 0.0253(18) 0.042(2) -0.0135(16) 0.0165(17) -0.0011(15) O2 0.0104(7) 0.0218(8) 0.0109(7) -0.0024(6) 0.0062(6) 0.0018(6) O3 0.0163(8) 0.0127(7) 0.0247(9) 0.0019(6) 0.0138(7) -0.0006(6) O4 0.0111(7) 0.0138(7) 0.0116(7) 0.0008(6) 0.0046(6) -0.0039(6) O5 0.0118(7) 0.0139(8) 0.0232(8) -0.0059(6) 0.0034(7) 0.0030(6) O6 0.0131(7) 0.0181(8) 0.0154(8) 0.0039(6) 0.0040(6) -0.0055(6) O7 0.0145(8) 0.0143(7) 0.0135(8) -0.0038(6) 0.0095(7) -0.0045(6) O8 0.0107(7) 0.0133(7) 0.0135(8) 0.0020(6) 0.0028(6) -0.0022(6) O9 0.0114(7) 0.0129(7) 0.0098(7) 0.0009(5) 0.0060(6) -0.0021(5) O10 0.0134(7) 0.0103(7) 0.0124(7) -0.0018(5) 0.0075(6) -0.0018(5) O11 0.0129(7) 0.0107(7) 0.0126(7) -0.0031(5) 0.0035(6) 0.0007(5) O12 0.0102(7) 0.0142(7) 0.0142(7) -0.0013(6) 0.0031(6) 0.0031(6) O13 0.0103(7) 0.0162(7) 0.0101(7) -0.0004(6) 0.0045(6) -0.0001(6) O14 0.0194(12) 0.0129(11) 0.0304(13) 0.000 0.0142(11) 0.000 O15 -0.001(5) 0.008(2) 0.021(3) -0.0044(18) 0.012(4) -0.007(3) O15A 0.004(6) 0.030(3) 0.033(3) -0.007(2) 0.017(4) -0.014(3) C1 0.0050(9) 0.0107(9) 0.0094(9) 0.0014(7) 0.0024(8) 0.0014(7) C1S 0.041(3) 0.031(3) 0.023(3) -0.011(2) 0.017(2) -0.010(2) C2 0.0095(9) 0.0075(9) 0.0107(9) 0.0032(7) 0.0052(8) 0.0019(7) C3 0.0111(10) 0.0103(9) 0.0115(10) 0.0016(7) 0.0078(8) -0.0007(7) C4 0.0089(9) 0.0093(9) 0.0049(9) -0.0002(7) 0.0031(8) -0.0012(7) C5 0.0081(9) 0.0118(9) 0.0046(9) -0.0002(7) 0.0027(8) 0.0001(7) C6 0.0081(9) 0.0109(9) 0.0045(9) 0.0004(7) 0.0013(7) 0.0003(7) C7 0.012(2) 0.024(2) 0.037(3) -0.006(2) 0.010(2) 0.001(2) _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 O6 2.0635(16) . ? Co1 O4 2.0716(14) . ? Co1 O3 2.0967(15) . ? Co1 O5 2.0997(15) . ? Co1 O15A 2.106(19) . ? Co1 O1 2.1066(14) . ? Co1 O15 2.120(15) . ? Co2 O8 2.0533(15) . ? Co2 O8 2.0534(15) 5_565 ? Co2 O7 2.0797(14) 5_565 ? Co2 O7 2.0798(14) . ? Co2 O9 2.2017(13) . ? Co2 O9 2.2017(13) 5_565 ? O1 C2 1.270(2) . ? O1S C1S 1.435(6) . ? O2 C2 1.250(2) . ? O9 C1 1.261(2) . ? O10 C1 1.259(2) . ? O11 C3 1.264(2) . ? O12 C3 1.248(2) . ? O15 C7 1.532(15) . ? C1 C4 1.514(3) . ? C1S C1S 1.831(11) 7_566 ? C2 C5 1.511(3) . ? C3 C6 1.513(3) . ? C4 C4 1.392(4) 2 ? C4 C5 1.400(3) . ? C5 C6 1.396(3) . ? C6 C6 1.402(4) 2 ? 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 O6 Co1 O4 179.13(6) . . ? O6 Co1 O3 90.21(6) . . ? O4 Co1 O3 88.92(6) . . ? O6 Co1 O5 93.68(7) . . ? O4 Co1 O5 86.34(6) . . ? O3 Co1 O5 93.63(7) . . ? O6 Co1 O15A 91.3(6) . . ? O4 Co1 O15A 88.7(6) . . ? O3 Co1 O15A 88.7(3) . . ? O5 Co1 O15A 174.5(5) . . ? O6 Co1 O1 92.19(6) . . ? O4 Co1 O1 88.69(6) . . ? O3 Co1 O1 176.05(6) . . ? O5 Co1 O1 89.35(6) . . ? O15A Co1 O1 88.1(3) . . ? O6 Co1 O15 92.0(5) . . ? O4 Co1 O15 87.9(5) . . ? O3 Co1 O15 80.3(3) . . ? O5 Co1 O15 171.7(4) . . ? O15A Co1 O15 8.5(6) . . ? O1 Co1 O15 96.5(3) . . ? O8 Co2 O8 180.0 . 5_565 ? O8 Co2 O7 83.99(6) . 5_565 ? O8 Co2 O7 96.01(6) 5_565 5_565 ? O8 Co2 O7 96.01(6) . . ? O8 Co2 O7 83.99(6) 5_565 . ? O7 Co2 O7 179.999(4) 5_565 . ? O8 Co2 O9 99.15(5) . . ? O8 Co2 O9 80.85(5) 5_565 . ? O7 Co2 O9 84.94(5) 5_565 . ? O7 Co2 O9 95.06(5) . . ? O8 Co2 O9 80.85(5) . 5_565 ? O8 Co2 O9 99.15(5) 5_565 5_565 ? O7 Co2 O9 95.06(5) 5_565 5_565 ? O7 Co2 O9 84.94(5) . 5_565 ? O9 Co2 O9 180.0 . 5_565 ? C2 O1 Co1 120.95(12) . . ? C1 O9 Co2 131.86(12) . . ? C7 O15 Co1 121.8(7) . . ? O10 C1 O9 125.10(17) . . ? O10 C1 C4 117.49(16) . . ? O9 C1 C4 117.42(16) . . ? O1S C1S C1S 110.0(5) . 7_566 ? O2 C2 O1 125.45(17) . . ? O2 C2 C5 118.40(16) . . ? O1 C2 C5 116.14(16) . . ? O12 C3 O11 126.28(18) . . ? O12 C3 C6 118.80(17) . . ? O11 C3 C6 114.91(16) . . ? C4 C4 C5 120.34(11) 2 . ? C4 C4 C1 120.25(10) 2 . ? C5 C4 C1 119.40(16) . . ? C6 C5 C4 119.45(17) . . ? C6 C5 C2 119.56(16) . . ? C4 C5 C2 120.99(16) . . ? C5 C6 C6 120.20(11) . 2 ? C5 C6 C3 120.43(16) . . ? C6 C6 C3 119.27(10) 2 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.441 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.068 data_2 _database_code_depnum_ccdc_archive 'CCDC 903327' #TrackingRef 'web_deposit_cif_file_1_SlaviSevov_1348603138.2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cobalt-mellitate _chemical_melting_point '[Co3(C6(COO)6)(H2O)5](H2O)' _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Co3 O18' _chemical_formula_weight 621.01 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' 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.165(4) _cell_length_b 9.0577(12) _cell_length_c 16.073(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.167(4) _cell_angle_gamma 90.00 _cell_volume 3462.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 2.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6521 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'Blessing, R.H. (1995) Acta Cryst. A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19396 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.40 _reflns_number_total 3528 _reflns_number_gt 3081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL-V5.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0292P)^2^+4.2574P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3528 _refine_ls_number_parameters 334 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.048 _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 0.371016(11) 0.74036(3) 0.997135(16) 0.00717(8) Uani 1 1 d . . . Co2 Co 0.292981(11) 0.73670(3) 0.792177(16) 0.00678(8) Uani 1 1 d . . . Co3 Co 0.430144(11) 0.24774(3) 0.873425(17) 0.00745(8) Uani 1 1 d . . . C1 C 0.48238(8) 0.6171(2) 0.78014(12) 0.0082(4) Uani 1 1 d . . . C2 C 0.46407(8) 0.7498(2) 0.81007(12) 0.0079(4) Uani 1 1 d . . . C3 C 0.48205(8) 0.8818(2) 0.77967(12) 0.0080(4) Uani 1 1 d . . . C4 C 0.46364(8) 0.4747(2) 0.81276(12) 0.0090(4) Uani 1 1 d . . . C5 C 0.42748(8) 0.75330(19) 0.87737(13) 0.0079(4) Uani 1 1 d . . . C6 C 0.46370(8) 1.0236(2) 0.81298(12) 0.0088(4) Uani 1 1 d . . . C7 C 0.27470(8) 0.2646(2) 0.92834(12) 0.0070(4) Uani 1 1 d . . . C8 C 0.25862(8) 0.3901(2) 0.96915(12) 0.0073(4) Uani 1 1 d . . . C9 C 0.23337(8) 0.3768(2) 1.04070(12) 0.0072(4) Uani 1 1 d . . . C10 C 0.30736(8) 0.2850(2) 0.85722(12) 0.0073(4) Uani 1 1 d . . . C11 C 0.27374(7) 0.5415(2) 0.93962(12) 0.0072(4) Uani 1 1 d . . . C12 C 0.20787(8) 0.5165(2) 1.07155(12) 0.0073(4) Uani 1 1 d . . . O1 O 0.43498(6) 0.38610(15) 0.76309(8) 0.0123(3) Uani 1 1 d . . . O2 O 0.47584(6) 0.44882(15) 0.89145(8) 0.0112(3) Uani 1 1 d . . . O3 O 0.37805(5) 0.69965(15) 0.86324(8) 0.0088(3) Uani 1 1 d . . . O4 O 0.44733(6) 0.80642(15) 0.94837(8) 0.0104(3) Uani 1 1 d . . . O5 O 0.41172(5) 1.04873(14) 0.80824(9) 0.0102(3) Uani 1 1 d . . . O6 O 0.49972(6) 1.11475(15) 0.84747(9) 0.0117(3) Uani 1 1 d . . . O7 O 0.35584(5) 0.34183(14) 0.88085(9) 0.0098(3) Uani 1 1 d . . . O8 O 0.28760(6) 0.24905(14) 0.78321(9) 0.0097(3) Uani 1 1 d . . . O9 O 0.26206(6) 0.57032(14) 0.86116(8) 0.0090(3) Uani 1 1 d . . . O10 O 0.29877(5) 0.62477(14) 0.99606(8) 0.0097(3) Uani 1 1 d . . . O11 O 0.22972(5) 0.57726(15) 1.14026(8) 0.0096(3) Uani 1 1 d . . . O12 O 0.16519(5) 0.55987(14) 1.02186(9) 0.0109(3) Uani 1 1 d . . . O1W O 0.39217(6) 0.79098(16) 1.12210(9) 0.0134(3) Uani 1 1 d D . . H1W H 0.3943(10) 0.7192(19) 1.1550(13) 0.020 Uiso 1 1 d D . . H2W H 0.4225(6) 0.837(2) 1.1330(15) 0.020 Uiso 1 1 d D . . O2W O 0.40928(6) 0.53189(16) 1.02737(9) 0.0132(3) Uani 1 1 d D . . H3W H 0.4442(4) 0.532(3) 1.0427(15) 0.020 Uiso 1 1 d D . . H4W H 0.4020(10) 0.473(2) 0.9869(11) 0.020 Uiso 1 1 d D . . O3W O 0.31931(6) 0.56752(15) 0.71950(9) 0.0108(3) Uani 1 1 d D . . H5W H 0.3411(8) 0.511(2) 0.7500(12) 0.016 Uiso 1 1 d D . . H6W H 0.2929(7) 0.517(2) 0.6934(13) 0.016 Uiso 1 1 d D . . O4W O 0.32383(6) 0.89801(15) 0.71857(9) 0.0098(3) Uani 1 1 d D . . H7W H 0.2997(8) 0.960(2) 0.6965(13) 0.015 Uiso 1 1 d D . . H8W H 0.3477(8) 0.952(2) 0.7473(13) 0.015 Uiso 1 1 d D . . O5W O 0.44175(6) 0.16551(17) 0.99064(9) 0.0148(3) Uani 1 1 d D . . H9W H 0.4755(5) 0.164(3) 1.0147(14) 0.022 Uiso 1 1 d D . . H10W H 0.4216(9) 0.201(3) 1.0231(13) 0.022 Uiso 1 1 d D . . O6W O 0.38413(8) 0.75021(17) 0.60705(11) 0.0226(4) Uani 1 1 d D . . H11W H 0.3766(11) 0.6605(13) 0.6135(17) 0.034 Uiso 1 1 d D . . H12W H 0.3642(10) 0.804(3) 0.6314(16) 0.034 Uiso 1 1 d 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 Co1 0.00735(14) 0.00719(14) 0.00705(14) -0.00006(10) 0.00145(10) 0.00019(9) Co2 0.00780(14) 0.00631(13) 0.00636(14) 0.00008(9) 0.00162(10) -0.00019(9) Co3 0.00757(14) 0.00661(14) 0.00853(14) -0.00026(10) 0.00243(10) 0.00006(10) C1 0.0074(9) 0.0096(9) 0.0068(9) 0.0001(7) -0.0013(7) -0.0005(7) C2 0.0053(9) 0.0113(10) 0.0066(9) -0.0003(7) -0.0006(7) 0.0002(7) C3 0.0059(9) 0.0094(9) 0.0082(9) -0.0003(7) 0.0000(7) 0.0004(7) C4 0.0063(9) 0.0086(9) 0.0129(10) -0.0003(8) 0.0043(8) 0.0032(7) C5 0.0097(9) 0.0037(9) 0.0102(10) 0.0027(7) 0.0018(8) 0.0031(7) C6 0.0119(10) 0.0094(9) 0.0057(9) 0.0028(7) 0.0033(7) -0.0005(7) C7 0.0052(9) 0.0095(9) 0.0057(9) -0.0011(7) -0.0011(7) 0.0004(7) C8 0.0062(9) 0.0074(9) 0.0070(9) 0.0010(7) -0.0024(7) -0.0007(7) C9 0.0060(9) 0.0081(9) 0.0068(9) -0.0005(7) -0.0011(7) 0.0011(7) C10 0.0086(9) 0.0027(8) 0.0106(10) 0.0022(7) 0.0020(8) 0.0031(7) C11 0.0042(8) 0.0059(9) 0.0121(10) 0.0003(7) 0.0036(7) 0.0026(7) C12 0.0066(9) 0.0080(9) 0.0088(10) 0.0020(7) 0.0054(7) -0.0023(7) O1 0.0169(7) 0.0106(7) 0.0100(7) -0.0018(6) 0.0038(6) -0.0044(6) O2 0.0123(7) 0.0114(7) 0.0094(7) 0.0021(6) 0.0008(5) -0.0012(6) O3 0.0078(7) 0.0095(7) 0.0095(7) -0.0002(5) 0.0024(5) -0.0002(5) O4 0.0100(7) 0.0125(7) 0.0088(7) -0.0014(5) 0.0017(5) 0.0003(5) O5 0.0074(7) 0.0100(7) 0.0129(7) -0.0024(6) 0.0012(5) 0.0008(5) O6 0.0113(7) 0.0097(7) 0.0148(7) -0.0040(6) 0.0044(6) -0.0020(5) O7 0.0079(7) 0.0096(7) 0.0122(7) -0.0022(5) 0.0023(5) -0.0002(5) O8 0.0106(7) 0.0114(7) 0.0075(7) -0.0006(5) 0.0027(6) 0.0007(5) O9 0.0115(7) 0.0082(6) 0.0076(7) 0.0016(5) 0.0027(5) -0.0005(5) O10 0.0102(7) 0.0096(7) 0.0101(7) -0.0022(5) 0.0034(5) -0.0032(5) O11 0.0122(7) 0.0084(7) 0.0083(7) -0.0007(5) 0.0019(6) 0.0009(5) O12 0.0113(7) 0.0082(7) 0.0121(7) -0.0005(6) -0.0007(6) 0.0025(5) O1W 0.0151(7) 0.0138(7) 0.0102(7) 0.0014(6) -0.0004(6) -0.0034(6) O2W 0.0130(7) 0.0128(7) 0.0135(8) 0.0000(6) 0.0021(6) 0.0026(6) O3W 0.0106(7) 0.0098(7) 0.0112(7) -0.0009(6) 0.0000(6) -0.0003(5) O4W 0.0092(7) 0.0093(7) 0.0102(7) 0.0002(6) 0.0000(6) -0.0007(5) O5W 0.0105(7) 0.0242(8) 0.0102(8) 0.0028(6) 0.0027(6) 0.0028(6) O6W 0.0285(9) 0.0198(9) 0.0235(9) -0.0012(7) 0.0156(8) 0.0005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O12 2.0096(13) 7_567 ? Co1 O10 2.0333(13) . ? Co1 O1W 2.0355(15) . ? Co1 O2W 2.1209(15) . ? Co1 O4 2.2098(14) . ? Co1 O3 2.2193(14) . ? Co2 O9 2.0860(13) . ? Co2 O3W 2.0927(14) . ? Co2 O4W 2.0979(14) . ? Co2 O8 2.1072(14) 4_556 ? Co2 O11 2.1283(14) 7_567 ? Co2 O3 2.1942(14) . ? Co3 O5W 1.9990(15) . ? Co3 O7 2.0102(13) . ? Co3 O5 2.0930(14) 1_545 ? Co3 O2 2.1231(14) . ? Co3 O6 2.1679(14) 1_545 ? Co3 O1 2.1915(14) . ? Co3 C6 2.449(2) 1_545 ? Co3 C4 2.472(2) . ? C1 C2 1.395(3) . ? C1 C1 1.398(4) 2_656 ? C1 C4 1.493(3) . ? C2 C3 1.389(3) . ? C2 C5 1.513(3) . ? C3 C3 1.398(4) 2_656 ? C3 C6 1.489(3) . ? C4 O1 1.251(2) . ? C4 O2 1.269(2) . ? C5 O4 1.253(2) . ? C5 O3 1.272(2) . ? C6 O6 1.255(2) . ? C6 O5 1.266(2) . ? C6 Co3 2.449(2) 1_565 ? C7 C9 1.400(3) 7_557 ? C7 C8 1.401(3) . ? C7 C10 1.511(3) . ? C8 C9 1.399(3) . ? C8 C11 1.516(3) . ? C9 C7 1.400(3) 7_557 ? C9 C12 1.528(3) . ? C10 O8 1.244(2) . ? C10 O7 1.274(2) . ? C11 O10 1.251(2) . ? C11 O9 1.270(2) . ? C12 O12 1.251(2) . ? C12 O11 1.263(2) . ? O5 Co3 2.0930(13) 1_565 ? O6 Co3 2.1679(14) 1_565 ? O8 Co2 2.1072(14) 4_546 ? O11 Co2 2.1284(14) 7_567 ? O12 Co1 2.0096(13) 7_567 ? O1W H1W 0.834(10) . ? O1W H2W 0.836(10) . ? O2W H3W 0.837(10) . ? O2W H4W 0.838(10) . ? O3W H5W 0.828(10) . ? O3W H6W 0.835(10) . ? O4W H7W 0.842(10) . ? O4W H8W 0.831(10) . ? O5W H9W 0.839(10) . ? O5W H10W 0.837(10) . ? O6W H11W 0.843(10) . ? O6W H12W 0.833(10) . ? 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 O12 Co1 O10 96.44(5) 7_567 . ? O12 Co1 O1W 88.51(6) 7_567 . ? O10 Co1 O1W 100.96(6) . . ? O12 Co1 O2W 175.54(6) 7_567 . ? O10 Co1 O2W 83.25(6) . . ? O1W Co1 O2W 87.19(6) . . ? O12 Co1 O4 94.04(5) 7_567 . ? O10 Co1 O4 154.89(5) . . ? O1W Co1 O4 102.06(6) . . ? O2W Co1 O4 87.99(6) . . ? O12 Co1 O3 96.20(5) 7_567 . ? O10 Co1 O3 96.82(5) . . ? O1W Co1 O3 160.98(6) . . ? O2W Co1 O3 88.24(5) . . ? O4 Co1 O3 59.30(5) . . ? O9 Co2 O3W 86.58(6) . . ? O9 Co2 O4W 177.64(5) . . ? O3W Co2 O4W 91.26(6) . . ? O9 Co2 O8 87.85(5) . 4_556 ? O3W Co2 O8 93.39(5) . 4_556 ? O4W Co2 O8 91.32(5) . 4_556 ? O9 Co2 O11 98.74(6) . 7_567 ? O3W Co2 O11 174.63(5) . 7_567 ? O4W Co2 O11 83.43(5) . 7_567 ? O8 Co2 O11 87.49(5) 4_556 7_567 ? O9 Co2 O3 90.20(5) . . ? O3W Co2 O3 80.18(5) . . ? O4W Co2 O3 90.38(5) . . ? O8 Co2 O3 173.38(5) 4_556 . ? O11 Co2 O3 99.07(5) 7_567 . ? O5W Co3 O7 94.60(6) . . ? O5W Co3 O5 97.64(6) . 1_545 ? O7 Co3 O5 106.35(5) . 1_545 ? O5W Co3 O2 102.00(6) . . ? O7 Co3 O2 94.40(5) . . ? O5 Co3 O2 150.08(5) 1_545 . ? O5W Co3 O6 89.42(6) . 1_545 ? O7 Co3 O6 168.04(5) . 1_545 ? O5 Co3 O6 61.88(5) 1_545 1_545 ? O2 Co3 O6 95.77(5) . 1_545 ? O5W Co3 O1 163.16(6) . . ? O7 Co3 O1 88.94(5) . . ? O5 Co3 O1 97.15(5) 1_545 . ? O2 Co3 O1 61.26(5) . . ? O6 Co3 O1 90.46(5) 1_545 . ? O5W Co3 C6 93.66(6) . 1_545 ? O7 Co3 C6 137.44(6) . 1_545 ? O5 Co3 C6 31.11(6) 1_545 1_545 ? O2 Co3 C6 124.36(6) . 1_545 ? O6 Co3 C6 30.78(6) 1_545 1_545 ? O1 Co3 C6 94.83(6) . 1_545 ? O5W Co3 C4 132.87(6) . . ? O7 Co3 C4 91.67(6) . . ? O5 Co3 C4 125.05(6) 1_545 . ? O2 Co3 C4 30.89(6) . . ? O6 Co3 C4 93.84(6) 1_545 . ? O1 Co3 C4 30.38(6) . . ? C6 Co3 C4 112.22(7) 1_545 . ? C2 C1 C1 120.52(11) . 2_656 ? C2 C1 C4 119.29(17) . . ? C1 C1 C4 120.19(10) 2_656 . ? C3 C2 C1 118.80(18) . . ? C3 C2 C5 119.47(16) . . ? C1 C2 C5 121.67(17) . . ? C2 C3 C3 120.68(11) . 2_656 ? C2 C3 C6 118.96(17) . . ? C3 C3 C6 120.34(10) 2_656 . ? O1 C4 O2 121.53(18) . . ? O1 C4 C1 119.87(17) . . ? O2 C4 C1 118.56(17) . . ? O1 C4 Co3 62.33(10) . . ? O2 C4 Co3 59.20(10) . . ? C1 C4 Co3 176.42(14) . . ? O4 C5 O3 120.36(18) . . ? O4 C5 C2 118.74(17) . . ? O3 C5 C2 120.87(17) . . ? O6 C6 O5 120.80(18) . . ? O6 C6 C3 119.92(17) . . ? O5 C6 C3 119.24(17) . . ? O6 C6 Co3 62.12(10) . 1_565 ? O5 C6 Co3 58.70(10) . 1_565 ? C3 C6 Co3 176.33(14) . 1_565 ? C9 C7 C8 120.54(18) 7_557 . ? C9 C7 C10 120.32(17) 7_557 . ? C8 C7 C10 118.71(17) . . ? C9 C8 C7 120.80(17) . . ? C9 C8 C11 119.97(16) . . ? C7 C8 C11 119.00(17) . . ? C8 C9 C7 118.65(17) . 7_557 ? C8 C9 C12 117.03(16) . . ? C7 C9 C12 123.57(17) 7_557 . ? O8 C10 O7 124.61(18) . . ? O8 C10 C7 121.86(17) . . ? O7 C10 C7 113.53(16) . . ? O10 C11 O9 126.19(18) . . ? O10 C11 C8 115.52(17) . . ? O9 C11 C8 118.24(16) . . ? O12 C12 O11 126.29(18) . . ? O12 C12 C9 112.77(16) . . ? O11 C12 C9 120.95(16) . . ? C4 O1 Co3 87.29(11) . . ? C4 O2 Co3 89.91(11) . . ? C5 O3 Co2 142.97(12) . . ? C5 O3 Co1 89.64(11) . . ? Co2 O3 Co1 104.73(5) . . ? C5 O4 Co1 90.56(12) . . ? C6 O5 Co3 90.19(11) . 1_565 ? C6 O6 Co3 87.10(11) . 1_565 ? C10 O7 Co3 126.50(12) . . ? C10 O8 Co2 136.32(13) . 4_546 ? C11 O9 Co2 129.70(12) . . ? C11 O10 Co1 128.42(12) . . ? C12 O11 Co2 133.27(12) . 7_567 ? C12 O12 Co1 131.86(13) . 7_567 ? Co1 O1W H1W 115.2(18) . . ? Co1 O1W H2W 112.3(17) . . ? H1W O1W H2W 108(2) . . ? Co1 O2W H3W 116.5(17) . . ? Co1 O2W H4W 111.6(17) . . ? H3W O2W H4W 107(2) . . ? Co2 O3W H5W 110.2(16) . . ? Co2 O3W H6W 113.5(17) . . ? H5W O3W H6W 108(2) . . ? Co2 O4W H7W 114.4(16) . . ? Co2 O4W H8W 112.2(16) . . ? H7W O4W H8W 102(2) . . ? Co3 O5W H9W 113.8(17) . . ? Co3 O5W H10W 116.5(18) . . ? H9W O5W H10W 110(2) . . ? H11W O6W H12W 111(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.424 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.072 data_1 _database_code_depnum_ccdc_archive 'CCDC 903328' #TrackingRef 'web_deposit_cif_file_2_SlaviSevov_1348603138.3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Co4(mel)(OH)2(H2O)]6(H2O)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Co4 O20' _chemical_formula_weight 713.95 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' 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.8707(17) _cell_length_b 6.4205(5) _cell_length_c 16.0526(13) _cell_angle_alpha 90.00 _cell_angle_beta 122.8270(10) _cell_angle_gamma 90.00 _cell_volume 1807.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4198 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.10 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.093 _exptl_crystal_size_mid 0.067 _exptl_crystal_size_min 0.063 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 3.726 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11627 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.21 _reflns_number_total 1815 _reflns_number_gt 1556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Diamond _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+4.3394P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1815 _refine_ls_number_parameters 185 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0473 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.058 _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 Co1 Co 0.039776(17) 0.45183(5) 0.11278(2) 0.00691(9) Uani 1 1 d . . . Co2 Co 0.155399(18) 0.73820(5) 0.09347(2) 0.00754(9) Uani 1 1 d . . . O1 O 0.13900(9) 0.4049(3) 0.10423(12) 0.0080(4) Uani 1 1 d . . . O1W O 0.06460(11) 0.1601(3) 0.18847(16) 0.0237(5) Uani 1 1 d D . . H1A H 0.0495(19) 0.233(5) 0.218(2) 0.036 Uiso 1 1 d D . . H1B H 0.0323(15) 0.070(4) 0.180(3) 0.036 Uiso 1 1 d D . . O2 O 0.14355(10) 0.0607(3) 0.10606(13) 0.0126(4) Uani 1 1 d . . . O2W O 0.27001(10) 0.7181(3) 0.14006(14) 0.0174(4) Uani 1 1 d D . . H2A H 0.2871(17) 0.724(5) 0.104(2) 0.026 Uiso 1 1 d D . . H2B H 0.3040(13) 0.704(5) 0.1996(9) 0.026 Uiso 1 1 d D . . O3 O 0.30026(10) 0.2451(3) 0.25666(13) 0.0132(4) Uani 1 1 d . . . O3W O 0.14356(10) 0.7796(3) -0.04589(14) 0.0110(4) Uani 1 1 d D . . H3A H 0.1180(14) 0.887(3) -0.0736(19) 0.016 Uiso 1 1 d D . . H3B H 0.1144(13) 0.680(3) -0.0778(19) 0.016 Uiso 1 1 d D . . O4 O 0.39440(10) 0.0912(3) 0.25243(13) 0.0144(4) Uani 1 1 d . . . O5 O 0.44876(10) 0.3837(3) 0.13184(14) 0.0175(4) Uani 1 1 d . . . O6 O 0.44576(9) 0.0369(3) 0.11843(12) 0.0098(4) Uani 1 1 d . . . O7 O 0.03652(10) 0.6987(3) 0.02618(13) 0.0091(4) Uani 1 1 d . . . H7 H 0.0183(17) 0.789(5) 0.029(2) 0.013(9) Uiso 1 1 d . . . C1 C 0.16293(13) 0.2348(4) 0.09163(17) 0.0073(5) Uani 1 1 d . . . C2 C 0.33155(13) 0.1807(4) 0.21321(18) 0.0072(5) Uani 1 1 d . . . C3 C 0.41542(13) 0.2133(4) 0.10957(17) 0.0078(5) Uani 1 1 d . . . C4 C 0.21043(13) 0.2445(4) 0.04666(18) 0.0059(5) Uani 1 1 d . . . C5 C 0.28937(13) 0.2159(4) 0.10321(18) 0.0060(5) Uani 1 1 d . . . C6 C 0.32900(13) 0.2220(3) 0.05514(18) 0.0059(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 Co1 0.00497(16) 0.00952(18) 0.00552(17) -0.00051(14) 0.00237(13) -0.00026(13) Co2 0.00791(17) 0.00827(17) 0.00694(18) -0.00007(14) 0.00434(14) -0.00080(13) O1 0.0082(8) 0.0075(9) 0.0106(9) -0.0003(7) 0.0067(8) 0.0014(6) O1W 0.0208(11) 0.0225(12) 0.0222(12) 0.0055(10) 0.0081(10) -0.0072(9) O2 0.0176(9) 0.0077(9) 0.0199(10) -0.0012(8) 0.0149(9) -0.0017(7) O2W 0.0104(9) 0.0296(12) 0.0107(10) 0.0011(9) 0.0048(8) 0.0004(8) O3 0.0135(9) 0.0190(10) 0.0075(9) 0.0005(8) 0.0059(8) 0.0061(8) O3W 0.0103(9) 0.0084(10) 0.0122(10) -0.0004(7) 0.0048(8) -0.0010(7) O4 0.0088(9) 0.0256(11) 0.0082(9) 0.0078(8) 0.0043(8) 0.0081(8) O5 0.0090(9) 0.0110(10) 0.0243(11) 0.0023(8) 0.0037(8) -0.0026(7) O6 0.0058(8) 0.0122(9) 0.0111(9) -0.0022(7) 0.0043(7) 0.0014(7) O7 0.0092(9) 0.0081(10) 0.0100(10) -0.0004(7) 0.0052(8) 0.0011(7) C1 0.0048(11) 0.0110(13) 0.0028(12) 0.0014(10) -0.0002(10) 0.0017(10) C2 0.0068(11) 0.0064(12) 0.0078(13) -0.0008(10) 0.0036(10) -0.0024(9) C3 0.0072(11) 0.0147(14) 0.0006(12) 0.0018(9) 0.0015(10) 0.0012(10) C4 0.0078(11) 0.0042(11) 0.0079(12) -0.0009(10) 0.0056(10) -0.0007(9) C5 0.0071(11) 0.0051(12) 0.0061(12) -0.0003(9) 0.0038(10) 0.0005(9) C6 0.0061(11) 0.0033(11) 0.0073(12) 0.0000(9) 0.0029(10) 0.0007(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 Co1 O4 2.0363(17) 4 ? Co1 O7 2.0848(18) . ? Co1 O6 2.0858(16) 3_455 ? Co1 O1W 2.138(2) . ? Co1 O7 2.1433(18) 5_565 ? Co1 O1 2.1694(16) . ? Co2 O3 2.0574(17) 4 ? Co2 O2W 2.0875(19) . ? Co2 O2 2.1082(18) 1_565 ? Co2 O7 2.1170(18) . ? Co2 O3W 2.1299(19) . ? Co2 O1 2.1889(17) . ? O1 C1 1.262(3) . ? O2 C1 1.252(3) . ? O2 Co2 2.1082(18) 1_545 ? O3 C2 1.256(3) . ? O3 Co2 2.0573(17) 4_545 ? O4 C2 1.246(3) . ? O4 Co1 2.0364(17) 4_545 ? O5 C3 1.241(3) . ? O6 C3 1.267(3) . ? O6 Co1 2.0857(16) 3_545 ? O7 Co1 2.1433(18) 5_565 ? C1 C4 1.511(3) . ? C2 C5 1.503(3) . ? C3 C6 1.520(3) . ? C4 C6 1.391(3) 7 ? C4 C5 1.397(3) . ? C5 C6 1.405(3) . ? C6 C4 1.391(3) 7 ? 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 O4 Co1 O7 97.69(7) 4 . ? O4 Co1 O6 86.98(7) 4 3_455 ? O7 Co1 O6 97.96(7) . 3_455 ? O4 Co1 O1W 87.99(8) 4 . ? O7 Co1 O1W 162.80(8) . . ? O6 Co1 O1W 98.55(7) 3_455 . ? O4 Co1 O7 175.24(7) 4 5_565 ? O7 Co1 O7 84.92(7) . 5_565 ? O6 Co1 O7 88.72(7) 3_455 5_565 ? O1W Co1 O7 90.63(8) . 5_565 ? O4 Co1 O1 90.63(7) 4 . ? O7 Co1 O1 75.56(7) . . ? O6 Co1 O1 172.75(7) 3_455 . ? O1W Co1 O1 88.21(7) . . ? O7 Co1 O1 93.88(7) 5_565 . ? O3 Co2 O2W 83.15(7) 4 . ? O3 Co2 O2 82.44(7) 4 1_565 ? O2W Co2 O2 101.40(7) . 1_565 ? O3 Co2 O7 105.01(7) 4 . ? O2W Co2 O7 166.84(8) . . ? O2 Co2 O7 90.04(7) 1_565 . ? O3 Co2 O3W 161.45(7) 4 . ? O2W Co2 O3W 80.92(7) . . ? O2 Co2 O3W 91.44(7) 1_565 . ? O7 Co2 O3W 92.43(7) . . ? O3 Co2 O1 85.37(7) 4 . ? O2W Co2 O1 96.26(7) . . ? O2 Co2 O1 157.12(6) 1_565 . ? O7 Co2 O1 74.51(7) . . ? O3W Co2 O1 105.72(7) . . ? C1 O1 Co1 127.22(15) . . ? C1 O1 Co2 137.81(15) . . ? Co1 O1 Co2 93.71(6) . . ? C1 O2 Co2 142.43(16) . 1_545 ? C2 O3 Co2 127.05(16) . 4_545 ? C2 O4 Co1 131.20(16) . 4_545 ? C3 O6 Co1 130.84(15) . 3_545 ? Co1 O7 Co2 98.36(8) . . ? Co1 O7 Co1 95.08(7) . 5_565 ? Co2 O7 Co1 126.09(9) . 5_565 ? O2 C1 O1 123.2(2) . . ? O2 C1 C4 119.1(2) . . ? O1 C1 C4 117.4(2) . . ? O4 C2 O3 126.4(2) . . ? O4 C2 C5 116.7(2) . . ? O3 C2 C5 116.9(2) . . ? O5 C3 O6 126.0(2) . . ? O5 C3 C6 116.0(2) . . ? O6 C3 C6 117.5(2) . . ? C6 C4 C5 121.5(2) 7 . ? C6 C4 C1 116.3(2) 7 . ? C5 C4 C1 122.2(2) . . ? C4 C5 C6 118.5(2) . . ? C4 C5 C2 121.1(2) . . ? C6 C5 C2 120.4(2) . . ? C4 C6 C5 120.0(2) 7 . ? C4 C6 C3 116.3(2) 7 . ? C5 C6 C3 123.5(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.21 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.700 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.084 data_1a _database_code_depnum_ccdc_archive 'CCDC 903329' #TrackingRef 'web_deposit_cif_file_3_SlaviSevov_1348603138.4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Mn-bpy-mellitate _chemical_melting_point ? _chemical_formula_moiety '[Mn4(Hmel)(H3mel)(bpy)4(H2O)8]' _chemical_formula_sum 'C64 H52.17 Mn4 N8 O32.08' _chemical_formula_weight 1666.43 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' 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 15.7969(8) _cell_length_b 20.9803(11) _cell_length_c 20.0682(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.453(2) _cell_angle_gamma 90.00 _cell_volume 6608.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 71.41 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.094 _exptl_crystal_size_mid 0.086 _exptl_crystal_size_min 0.057 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3395 _exptl_absorpt_coefficient_mu 6.980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.672 _exptl_absorpt_process_details 'Blessing, R.H. (1995) Acta Cryst. A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 78400 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 71.41 _reflns_number_total 12306 _reflns_number_gt 10717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL-V5.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0298P)^2^+6.1238P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12306 _refine_ls_number_parameters 1030 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.74617(2) 0.233527(15) 0.161712(16) 0.01153(7) Uani 1 1 d . . . Mn2 Mn 0.74379(2) 0.245515(15) 0.368687(16) 0.01049(7) Uani 1 1 d . . . Mn3 Mn 0.23044(2) 0.482880(15) 0.160350(16) 0.01131(7) Uani 1 1 d . . . Mn4 Mn 0.22817(2) 0.502978(15) 0.364801(16) 0.01046(7) Uani 1 1 d . . . O1 O 0.72703(9) 0.33385(7) 0.31274(7) 0.0148(3) Uani 1 1 d . . . O1W O 0.60819(10) 0.25690(7) 0.15940(8) 0.0182(3) Uani 1 1 d D . . H1WA H 0.5739(15) 0.2343(12) 0.1779(13) 0.027 Uiso 1 1 d D . . H1WB H 0.5969(17) 0.2944(6) 0.1697(14) 0.027 Uiso 1 1 d D . . O1S O -0.0431(13) 0.4763(10) 0.0949(10) 0.029(7) Uiso 0.088(6) 1 d P . . O2 O 0.77676(9) 0.31892(7) 0.21364(7) 0.0157(3) Uani 1 1 d . . . O2W O 0.88186(10) 0.20391(8) 0.17570(8) 0.0181(3) Uani 1 1 d D . . H2WA H 0.9230(13) 0.2292(11) 0.1823(14) 0.027 Uiso 1 1 d D . . H2WB H 0.8948(17) 0.1731(9) 0.2013(12) 0.027 Uiso 1 1 d D . . O3 O 0.56915(9) 0.37877(7) 0.19556(8) 0.0175(3) Uani 1 1 d . . . O3W O 0.61213(10) 0.22600(8) 0.33248(8) 0.0190(3) Uani 1 1 d D . . H3WA H 0.5702(13) 0.2508(11) 0.3302(14) 0.029 Uiso 1 1 d D . . H3WB H 0.5984(17) 0.1951(10) 0.3071(12) 0.029 Uiso 1 1 d D . . O4 O 0.55138(9) 0.43241(7) 0.28963(7) 0.0143(3) Uani 1 1 d . . . H4 H 0.5069 0.4102 0.2884 0.021 Uiso 1 1 calc R . . O4W O 0.87712(10) 0.25276(8) 0.33997(8) 0.0190(3) Uani 1 1 d D . . H4WA H 0.8925(17) 0.2190(8) 0.3228(13) 0.029 Uiso 1 1 d D . . H4WB H 0.8919(17) 0.2836(9) 0.3175(12) 0.029 Uiso 1 1 d D . . O5 O 0.52666(9) 0.52361(7) 0.17676(8) 0.0184(3) Uani 1 1 d . . . O6 O 0.58167(9) 0.61429(7) 0.22152(8) 0.0170(3) Uani 1 1 d . . . O6W O 0.36636(10) 0.46002(8) 0.17820(8) 0.0202(3) Uani 1 1 d D . . H6WA H 0.4099(12) 0.4824(12) 0.1749(15) 0.030 Uiso 1 1 d D . . H6WB H 0.3798(17) 0.4303(10) 0.2052(12) 0.030 Uiso 1 1 d D . . O7 O 0.73676(9) 0.64736(7) 0.15872(7) 0.0140(3) Uani 1 1 d . . . O7W O 0.09577(9) 0.47859(7) 0.33195(8) 0.0168(3) Uani 1 1 d D . . H7WA H 0.0574(13) 0.5061(10) 0.3254(14) 0.025 Uiso 1 1 d D . . H7WB H 0.0866(17) 0.4497(10) 0.3030(11) 0.025 Uiso 1 1 d D . . O8 O 0.77339(9) 0.66080(7) 0.26883(8) 0.0160(3) Uani 1 1 d . . . O8W O 0.36293(10) 0.50666(7) 0.34114(8) 0.0180(3) Uani 1 1 d D . . H8WA H 0.3831(17) 0.5382(9) 0.3225(13) 0.027 Uiso 1 1 d D . . H8WB H 0.3763(17) 0.4727(8) 0.3233(13) 0.027 Uiso 1 1 d D . . O9 O 0.92150(9) 0.59497(7) 0.20034(7) 0.0154(3) Uani 1 1 d . . . O10 O 0.95575(9) 0.55364(7) 0.30277(8) 0.0175(3) Uani 1 1 d . . . O11 O 0.92270(9) 0.37996(7) 0.29887(7) 0.0147(3) Uani 1 1 d . . . O12 O 0.96382(9) 0.43924(7) 0.21574(8) 0.0185(3) Uani 1 1 d . . . O13 O 0.20958(9) 0.58629(7) 0.30283(7) 0.0162(3) Uani 1 1 d . . . O14 O 0.25468(9) 0.57477(7) 0.20151(7) 0.0157(3) Uani 1 1 d . . . O15 O 0.06262(9) 0.64064(7) 0.19852(8) 0.0153(3) Uani 1 1 d . . . H15 H 0.0141 0.6265 0.2040 0.023 Uiso 1 1 calc R . . O16 O 0.03671(9) 0.70776(7) 0.28067(8) 0.0170(3) Uani 1 1 d . . . O17 O 0.09342(9) 0.87875(7) 0.21972(7) 0.0150(3) Uani 1 1 d . . . O18 O 0.03731(9) 0.79381(7) 0.16435(8) 0.0197(3) Uani 1 1 d . . . O19 O 0.25152(9) 0.90315(7) 0.15725(7) 0.0133(3) Uani 1 1 d . . . O20 O 0.29162(9) 0.91301(7) 0.26721(7) 0.0151(3) Uani 1 1 d . . . O21 O 0.43103(9) 0.83899(7) 0.19606(7) 0.0148(3) Uani 1 1 d . . . H21 H 0.4820 0.8511 0.2014 0.022 Uiso 1 1 calc R . . O22 O 0.47175(9) 0.77915(7) 0.28669(8) 0.0185(3) Uani 1 1 d . . . O23 O 0.44064(9) 0.66741(7) 0.19625(7) 0.0159(3) Uani 1 1 d . . . H23 H 0.4875 0.6486 0.2049 0.024 Uiso 1 1 calc R . . O24 O 0.41143(9) 0.62472(7) 0.29354(8) 0.0166(3) Uani 1 1 d . . . N1 N 0.70076(12) 0.17203(9) 0.07421(9) 0.0173(4) Uani 1 1 d . . . N2 N 0.77837(12) 0.28523(9) 0.06808(9) 0.0183(4) Uani 1 1 d . . . N3 N 0.68571(11) 0.30025(9) 0.44944(9) 0.0146(4) Uani 1 1 d . . . N4 N 0.80450(12) 0.21162(9) 0.47175(9) 0.0168(4) Uani 1 1 d . . . N5 N 0.17710(12) 0.41615(9) 0.07868(9) 0.0180(4) Uani 1 1 d . . . N6 N 0.27040(12) 0.52017(9) 0.06290(9) 0.0176(4) Uani 1 1 d . . . N7 N 0.28528(12) 0.47550(9) 0.47039(9) 0.0168(4) Uani 1 1 d . . . N8 N 0.17331(12) 0.56813(9) 0.43958(9) 0.0160(4) Uani 1 1 d . . . C1 C 0.75094(12) 0.35241(10) 0.25884(10) 0.0117(4) Uani 1 1 d . . . C2 C 0.59139(13) 0.41891(9) 0.23748(10) 0.0117(4) Uani 1 1 d . . . C3 C 0.58548(13) 0.55493(10) 0.20595(10) 0.0117(4) Uani 1 1 d . . . C4 C 0.75093(12) 0.62757(10) 0.21791(10) 0.0112(4) Uani 1 1 d . . . C5 C 0.90795(13) 0.55956(9) 0.25030(10) 0.0123(4) Uani 1 1 d . . . C6 C 0.91146(13) 0.42327(9) 0.25341(11) 0.0127(4) Uani 1 1 d . . . C7 C 0.74995(13) 0.42368(10) 0.24741(10) 0.0108(4) Uani 1 1 d . . . C8 C 0.67240(12) 0.45673(10) 0.23631(10) 0.0103(4) Uani 1 1 d . . . C9 C 0.67039(12) 0.52230(10) 0.22498(10) 0.0108(4) Uani 1 1 d . . . C10 C 0.74727(13) 0.55604(10) 0.22874(10) 0.0109(4) Uani 1 1 d . . . C11 C 0.82464(13) 0.52355(10) 0.24167(10) 0.0106(4) Uani 1 1 d . . . C12 C 0.82649(13) 0.45734(10) 0.24817(10) 0.0109(4) Uani 1 1 d . . . C13 C 0.23367(12) 0.60668(10) 0.24988(10) 0.0116(4) Uani 1 1 d . . . C14 C 0.08127(13) 0.68779(10) 0.23918(10) 0.0120(4) Uani 1 1 d . . . C15 C 0.09495(13) 0.82073(10) 0.20022(10) 0.0117(4) Uani 1 1 d . . . C16 C 0.26668(12) 0.88139(9) 0.21526(10) 0.0109(4) Uani 1 1 d . . . C17 C 0.41851(13) 0.79791(9) 0.24177(10) 0.0120(4) Uani 1 1 d . . . C18 C 0.39629(12) 0.66187(9) 0.24724(10) 0.0114(4) Uani 1 1 d . . . C19 C 0.23979(13) 0.67849(10) 0.24217(10) 0.0105(4) Uani 1 1 d . . . C20 C 0.16744(12) 0.71721(10) 0.23351(10) 0.0106(4) Uani 1 1 d . . . C21 C 0.17521(12) 0.78249(9) 0.22158(10) 0.0100(4) Uani 1 1 d . . . C22 C 0.25639(13) 0.81027(9) 0.22457(9) 0.0102(4) Uani 1 1 d . . . C23 C 0.32908(13) 0.77123(10) 0.23598(10) 0.0106(4) Uani 1 1 d . . . C24 C 0.32001(12) 0.70556(10) 0.24206(9) 0.0100(4) Uani 1 1 d . . . C25 C 0.65442(15) 0.11943(11) 0.08030(12) 0.0209(5) Uani 1 1 d . . . H25A H 0.6527 0.1017 0.1237 0.025 Uiso 1 1 calc R . . C26 C 0.60880(15) 0.08976(12) 0.02599(13) 0.0252(5) Uani 1 1 d . . . H26A H 0.5772 0.0520 0.0318 0.030 Uiso 1 1 calc R . . C27 C 0.61028(16) 0.11638(13) -0.03699(13) 0.0288(6) Uani 1 1 d . . . H27A H 0.5788 0.0975 -0.0751 0.035 Uiso 1 1 calc R . . C28 C 0.65807(16) 0.17081(13) -0.04401(12) 0.0265(5) Uani 1 1 d . . . H28A H 0.6599 0.1897 -0.0869 0.032 Uiso 1 1 calc R . . C29 C 0.70315(14) 0.19736(11) 0.01253(11) 0.0197(5) Uani 1 1 d . . . C30 C 0.75746(14) 0.25470(12) 0.00930(11) 0.0205(5) Uani 1 1 d . . . C31 C 0.78720(17) 0.27557(14) -0.04987(12) 0.0304(6) Uani 1 1 d . . . H31A H 0.7725 0.2531 -0.0906 0.036 Uiso 1 1 calc R . . C32 C 0.83814(18) 0.32914(14) -0.04862(14) 0.0347(6) Uani 1 1 d . . . H32A H 0.8587 0.3441 -0.0885 0.042 Uiso 1 1 calc R . . C33 C 0.85875(16) 0.36077(13) 0.01153(13) 0.0282(6) Uani 1 1 d . . . H33A H 0.8935 0.3978 0.0137 0.034 Uiso 1 1 calc R . . C34 C 0.82771(15) 0.33726(12) 0.06840(12) 0.0229(5) Uani 1 1 d . . . H34A H 0.8420 0.3590 0.1097 0.027 Uiso 1 1 calc R . . C35 C 0.62361(14) 0.34323(10) 0.43398(11) 0.0173(4) Uani 1 1 d . . . H35A H 0.6068 0.3526 0.3881 0.021 Uiso 1 1 calc R . . C36 C 0.58306(15) 0.37455(12) 0.48223(12) 0.0221(5) Uani 1 1 d . . . H36A H 0.5393 0.4047 0.4697 0.026 Uiso 1 1 calc R . . C37 C 0.60769(15) 0.36091(12) 0.54888(12) 0.0247(5) Uani 1 1 d . . . H37A H 0.5810 0.3816 0.5831 0.030 Uiso 1 1 calc R . . C38 C 0.67192(15) 0.31661(12) 0.56544(11) 0.0220(5) Uani 1 1 d . . . H38A H 0.6898 0.3067 0.6111 0.026 Uiso 1 1 calc R . . C39 C 0.70985(14) 0.28683(10) 0.51431(11) 0.0157(4) Uani 1 1 d . . . C40 C 0.77876(14) 0.23895(10) 0.52703(11) 0.0162(4) Uani 1 1 d . . . C41 C 0.81679(15) 0.22420(11) 0.59110(11) 0.0220(5) Uani 1 1 d . . . H41A H 0.7981 0.2443 0.6293 0.026 Uiso 1 1 calc R . . C42 C 0.88215(16) 0.17997(12) 0.59865(12) 0.0251(5) Uani 1 1 d . . . H42A H 0.9094 0.1698 0.6420 0.030 Uiso 1 1 calc R . . C43 C 0.90726(15) 0.15079(12) 0.54238(13) 0.0256(5) Uani 1 1 d . . . H43A H 0.9510 0.1195 0.5463 0.031 Uiso 1 1 calc R . . C44 C 0.86723(15) 0.16818(11) 0.47993(12) 0.0225(5) Uani 1 1 d . . . H44A H 0.8850 0.1485 0.4412 0.027 Uiso 1 1 calc R . . C45 C 0.12206(15) 0.36962(11) 0.08905(12) 0.0215(5) Uani 1 1 d . . . H45A H 0.1152 0.3581 0.1339 0.026 Uiso 1 1 calc R . . C46 C 0.07459(15) 0.33752(12) 0.03707(13) 0.0260(5) Uani 1 1 d . . . H46A H 0.0362 0.3046 0.0461 0.031 Uiso 1 1 calc R . . C47 C 0.08447(16) 0.35452(13) -0.02774(13) 0.0303(6) Uani 1 1 d . . . H47A H 0.0523 0.3337 -0.0643 0.036 Uiso 1 1 calc R . . C48 C 0.14163(16) 0.40218(13) -0.03947(12) 0.0282(6) Uani 1 1 d . . . H48A H 0.1494 0.4143 -0.0840 0.034 Uiso 1 1 calc R . . C49 C 0.18752(14) 0.43197(11) 0.01520(11) 0.0188(5) Uani 1 1 d . . . C50 C 0.24930(15) 0.48439(11) 0.00749(11) 0.0199(5) Uani 1 1 d . . . C51 C 0.28579(17) 0.49508(14) -0.05138(12) 0.0303(6) Uani 1 1 d . . . H51A H 0.2711 0.4690 -0.0897 0.036 Uiso 1 1 calc R . . C52 C 0.34377(18) 0.54422(15) -0.05341(13) 0.0356(7) Uani 1 1 d . . . H52A H 0.3693 0.5523 -0.0932 0.043 Uiso 1 1 calc R . . C53 C 0.36424(17) 0.58143(13) 0.00266(13) 0.0298(6) Uani 1 1 d . . . H53A H 0.4034 0.6158 0.0020 0.036 Uiso 1 1 calc R . . C54 C 0.32647(15) 0.56761(11) 0.05989(12) 0.0216(5) Uani 1 1 d . . . H54A H 0.3410 0.5929 0.0988 0.026 Uiso 1 1 calc R . . C55 C 0.34259(14) 0.42870(11) 0.48314(11) 0.0198(5) Uani 1 1 d . . . H55A H 0.3562 0.4030 0.4468 0.024 Uiso 1 1 calc R . . C56 C 0.38287(15) 0.41597(12) 0.54662(12) 0.0240(5) Uani 1 1 d . . . H56A H 0.4219 0.3816 0.5539 0.029 Uiso 1 1 calc R . . C57 C 0.36496(16) 0.45440(12) 0.59906(12) 0.0255(5) Uani 1 1 d . . . H57A H 0.3931 0.4478 0.6429 0.031 Uiso 1 1 calc R . . C58 C 0.30555(16) 0.50261(12) 0.58708(12) 0.0236(5) Uani 1 1 d . . . H58A H 0.2924 0.5295 0.6226 0.028 Uiso 1 1 calc R . . C59 C 0.26516(14) 0.51121(11) 0.52225(11) 0.0170(4) Uani 1 1 d . . . C60 C 0.19770(14) 0.55981(10) 0.50532(11) 0.0164(4) Uani 1 1 d . . . C61 C 0.16089(15) 0.59413(12) 0.55404(12) 0.0224(5) Uani 1 1 d . . . H61A H 0.1777 0.5866 0.6003 0.027 Uiso 1 1 calc R . . C62 C 0.09934(15) 0.63941(12) 0.53394(12) 0.0236(5) Uani 1 1 d . . . H62A H 0.0737 0.6636 0.5663 0.028 Uiso 1 1 calc R . . C63 C 0.07582(14) 0.64896(11) 0.46627(12) 0.0215(5) Uani 1 1 d . . . H63A H 0.0345 0.6802 0.4513 0.026 Uiso 1 1 calc R . . C64 C 0.11367(14) 0.61203(11) 0.42061(12) 0.0186(5) Uani 1 1 d . . . H64A H 0.0967 0.6180 0.3741 0.022 Uiso 1 1 calc R . . O5W O 0.09398(11) 0.51239(8) 0.15738(9) 0.0241(4) Uani 1 1 d D . . H5WA H 0.0900(19) 0.5514(6) 0.1658(15) 0.036 Uiso 1 1 d D . . H5WB H 0.0508(13) 0.4933(13) 0.1692(15) 0.036 Uiso 1 1 d 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 0.01410(17) 0.01021(16) 0.01019(16) -0.00020(12) 0.00091(11) 0.00023(12) Mn2 0.01128(17) 0.00916(16) 0.01084(16) 0.00016(12) 0.00038(11) -0.00028(11) Mn3 0.01395(17) 0.00941(16) 0.01039(16) -0.00027(12) 0.00057(11) 0.00058(11) Mn4 0.01169(17) 0.00911(16) 0.01054(16) -0.00025(12) 0.00096(11) -0.00036(11) O1 0.0152(8) 0.0132(7) 0.0167(8) 0.0043(6) 0.0049(6) 0.0002(5) O1W 0.0163(8) 0.0133(8) 0.0254(9) -0.0016(6) 0.0047(6) 0.0005(6) O2 0.0180(8) 0.0122(7) 0.0173(8) -0.0037(6) 0.0039(6) -0.0004(6) O2W 0.0141(8) 0.0170(8) 0.0223(8) 0.0028(6) -0.0011(6) -0.0006(6) O3 0.0152(8) 0.0144(8) 0.0228(8) -0.0047(6) 0.0013(6) -0.0011(6) O3W 0.0130(8) 0.0161(8) 0.0269(9) -0.0066(6) -0.0025(6) -0.0003(6) O4 0.0092(8) 0.0175(8) 0.0166(8) 0.0001(6) 0.0025(5) -0.0045(5) O4W 0.0171(8) 0.0182(8) 0.0223(9) 0.0030(6) 0.0046(6) 0.0001(6) O5 0.0120(8) 0.0158(8) 0.0262(9) 0.0000(6) -0.0035(6) 0.0000(6) O6 0.0112(8) 0.0135(8) 0.0259(8) -0.0046(6) -0.0004(6) 0.0036(5) O6W 0.0140(8) 0.0195(9) 0.0265(9) 0.0076(7) -0.0003(6) 0.0003(6) O7 0.0151(8) 0.0118(7) 0.0145(7) 0.0022(6) -0.0003(5) 0.0002(5) O7W 0.0140(8) 0.0142(8) 0.0212(8) -0.0028(6) -0.0026(6) 0.0017(6) O8 0.0163(8) 0.0131(7) 0.0181(8) -0.0047(6) -0.0009(6) 0.0002(6) O8W 0.0178(8) 0.0136(8) 0.0237(9) 0.0008(6) 0.0068(6) -0.0001(6) O9 0.0118(8) 0.0147(7) 0.0196(8) 0.0031(6) 0.0010(6) -0.0037(5) O10 0.0118(8) 0.0190(8) 0.0202(8) 0.0001(6) -0.0041(6) 0.0001(6) O11 0.0117(8) 0.0133(7) 0.0190(8) 0.0018(6) 0.0016(5) 0.0022(5) O12 0.0131(8) 0.0167(8) 0.0268(9) 0.0027(6) 0.0073(6) 0.0018(6) O13 0.0178(8) 0.0130(8) 0.0189(8) 0.0038(6) 0.0066(6) 0.0012(6) O14 0.0180(8) 0.0104(7) 0.0192(8) -0.0035(6) 0.0048(6) -0.0016(5) O15 0.0091(8) 0.0139(7) 0.0233(8) -0.0033(6) 0.0037(6) -0.0035(5) O16 0.0132(8) 0.0168(8) 0.0223(8) -0.0025(6) 0.0076(6) -0.0005(6) O17 0.0106(8) 0.0141(7) 0.0201(8) -0.0033(6) 0.0001(5) 0.0025(5) O18 0.0134(8) 0.0161(8) 0.0277(9) -0.0005(6) -0.0060(6) -0.0005(6) O19 0.0124(8) 0.0117(7) 0.0157(7) 0.0029(6) 0.0008(5) 0.0004(5) O20 0.0155(8) 0.0134(7) 0.0162(8) -0.0039(6) 0.0006(6) -0.0008(5) O21 0.0086(7) 0.0153(7) 0.0201(8) 0.0020(6) 0.0008(5) -0.0030(5) O22 0.0125(8) 0.0172(8) 0.0245(8) 0.0036(6) -0.0039(6) -0.0007(6) O23 0.0112(8) 0.0177(8) 0.0194(8) 0.0018(6) 0.0047(6) 0.0052(6) O24 0.0155(8) 0.0136(8) 0.0206(8) 0.0049(6) 0.0009(6) 0.0021(6) N1 0.0168(10) 0.0188(10) 0.0161(9) -0.0029(7) 0.0001(7) 0.0035(7) N2 0.0168(10) 0.0217(10) 0.0167(10) 0.0028(7) 0.0036(7) 0.0032(7) N3 0.0153(10) 0.0153(9) 0.0128(9) -0.0004(7) 0.0005(7) -0.0024(7) N4 0.0176(10) 0.0170(9) 0.0152(9) 0.0011(7) -0.0002(7) 0.0003(7) N5 0.0195(10) 0.0166(9) 0.0174(10) -0.0030(7) -0.0004(7) 0.0025(7) N6 0.0198(10) 0.0186(10) 0.0146(9) 0.0015(7) 0.0021(7) 0.0020(7) N7 0.0183(10) 0.0190(10) 0.0130(9) -0.0011(7) 0.0014(7) -0.0023(7) N8 0.0177(10) 0.0153(9) 0.0152(9) -0.0024(7) 0.0025(7) -0.0036(7) C1 0.0068(10) 0.0125(10) 0.0155(10) 0.0004(8) -0.0012(7) -0.0014(7) C2 0.0097(11) 0.0090(10) 0.0161(10) 0.0020(8) -0.0002(7) 0.0011(7) C3 0.0112(11) 0.0134(10) 0.0107(10) 0.0035(8) 0.0024(7) 0.0012(7) C4 0.0047(10) 0.0118(10) 0.0171(11) -0.0006(8) 0.0017(7) 0.0014(7) C5 0.0109(11) 0.0086(10) 0.0179(11) -0.0021(8) 0.0029(8) 0.0019(7) C6 0.0114(11) 0.0079(9) 0.0185(11) -0.0040(8) 0.0002(8) -0.0012(7) C7 0.0125(11) 0.0119(10) 0.0081(9) -0.0009(7) 0.0018(7) 0.0000(7) C8 0.0099(10) 0.0125(10) 0.0090(9) -0.0005(7) 0.0027(7) -0.0006(7) C9 0.0102(10) 0.0139(10) 0.0083(9) -0.0013(7) 0.0008(7) 0.0001(7) C10 0.0135(11) 0.0111(10) 0.0082(9) -0.0006(7) 0.0017(7) 0.0010(7) C11 0.0115(10) 0.0112(10) 0.0092(9) 0.0007(7) 0.0022(7) -0.0009(7) C12 0.0119(11) 0.0115(10) 0.0094(10) -0.0001(7) 0.0012(7) 0.0009(7) C13 0.0052(10) 0.0118(10) 0.0174(11) 0.0001(8) -0.0002(7) -0.0001(7) C14 0.0111(11) 0.0102(10) 0.0148(10) 0.0041(8) 0.0010(7) 0.0001(7) C15 0.0093(10) 0.0130(10) 0.0130(10) 0.0021(8) 0.0026(7) 0.0003(7) C16 0.0059(10) 0.0106(10) 0.0166(10) 0.0000(8) 0.0023(7) 0.0010(7) C17 0.0104(11) 0.0109(10) 0.0148(10) -0.0023(8) 0.0026(7) 0.0009(7) C18 0.0089(10) 0.0081(9) 0.0166(10) -0.0018(8) -0.0011(7) -0.0007(7) C19 0.0138(11) 0.0100(10) 0.0077(9) 0.0002(7) 0.0010(7) 0.0002(7) C20 0.0101(10) 0.0119(10) 0.0099(9) -0.0015(7) 0.0022(7) -0.0014(7) C21 0.0092(10) 0.0111(10) 0.0097(9) -0.0005(7) 0.0007(7) 0.0009(7) C22 0.0129(11) 0.0103(10) 0.0076(9) -0.0016(7) 0.0014(7) -0.0004(7) C23 0.0113(10) 0.0112(10) 0.0095(9) -0.0002(7) 0.0018(7) -0.0007(7) C24 0.0098(10) 0.0126(10) 0.0080(9) -0.0001(7) 0.0019(7) 0.0012(7) C25 0.0192(12) 0.0193(12) 0.0240(12) -0.0052(9) 0.0019(9) 0.0039(9) C26 0.0165(13) 0.0244(13) 0.0340(14) -0.0128(10) -0.0010(9) 0.0051(9) C27 0.0228(14) 0.0357(15) 0.0266(14) -0.0171(11) -0.0029(9) 0.0082(10) C28 0.0246(14) 0.0372(15) 0.0173(12) -0.0072(10) 0.0000(9) 0.0080(10) C29 0.0176(12) 0.0264(12) 0.0151(11) -0.0041(9) 0.0022(8) 0.0081(9) C30 0.0175(12) 0.0291(13) 0.0152(11) 0.0037(9) 0.0029(8) 0.0084(9) C31 0.0313(15) 0.0451(17) 0.0155(12) 0.0031(11) 0.0055(10) 0.0049(11) C32 0.0346(16) 0.0464(17) 0.0252(14) 0.0145(12) 0.0131(11) 0.0026(12) C33 0.0233(14) 0.0329(14) 0.0291(14) 0.0130(11) 0.0054(10) 0.0002(10) C34 0.0224(13) 0.0245(13) 0.0219(12) 0.0061(10) 0.0029(9) 0.0017(9) C35 0.0158(12) 0.0181(11) 0.0177(11) -0.0005(9) 0.0005(8) -0.0008(8) C36 0.0180(12) 0.0244(12) 0.0241(12) -0.0062(10) 0.0035(9) 0.0010(9) C37 0.0224(13) 0.0310(14) 0.0218(12) -0.0087(10) 0.0067(9) -0.0006(10) C38 0.0235(13) 0.0281(13) 0.0143(11) -0.0046(9) 0.0021(9) -0.0034(9) C39 0.0156(11) 0.0157(11) 0.0156(11) -0.0016(8) 0.0004(8) -0.0052(8) C40 0.0172(12) 0.0153(11) 0.0153(11) 0.0014(8) -0.0015(8) -0.0058(8) C41 0.0288(14) 0.0212(12) 0.0153(11) 0.0027(9) -0.0010(9) -0.0038(9) C42 0.0287(14) 0.0249(13) 0.0197(12) 0.0084(10) -0.0066(9) -0.0049(10) C43 0.0219(13) 0.0248(13) 0.0285(13) 0.0080(10) -0.0038(9) 0.0031(9) C44 0.0215(13) 0.0231(12) 0.0226(12) 0.0015(9) 0.0005(9) 0.0017(9) C45 0.0230(13) 0.0179(12) 0.0226(12) -0.0016(9) -0.0012(9) -0.0003(9) C46 0.0187(13) 0.0220(13) 0.0359(15) -0.0106(10) -0.0028(10) 0.0004(9) C47 0.0201(14) 0.0401(16) 0.0289(14) -0.0195(12) -0.0048(10) 0.0011(10) C48 0.0231(14) 0.0433(16) 0.0175(12) -0.0109(11) -0.0001(9) 0.0032(11) C49 0.0156(12) 0.0245(12) 0.0162(11) -0.0045(9) 0.0009(8) 0.0064(9) C50 0.0201(12) 0.0261(12) 0.0132(11) -0.0013(9) -0.0002(8) 0.0046(9) C51 0.0331(15) 0.0437(16) 0.0150(12) -0.0049(11) 0.0057(10) -0.0010(11) C52 0.0358(16) 0.0552(19) 0.0181(13) 0.0043(12) 0.0127(10) -0.0057(13) C53 0.0290(15) 0.0362(15) 0.0251(14) 0.0062(11) 0.0066(10) -0.0054(11) C54 0.0229(13) 0.0231(12) 0.0188(12) 0.0014(9) 0.0030(9) -0.0009(9) C55 0.0186(12) 0.0243(12) 0.0164(11) -0.0012(9) 0.0019(8) -0.0001(9) C56 0.0202(13) 0.0286(13) 0.0228(12) 0.0057(10) -0.0001(9) -0.0016(9) C57 0.0279(14) 0.0330(14) 0.0142(11) 0.0053(10) -0.0041(9) -0.0042(10) C58 0.0296(14) 0.0262(13) 0.0149(11) -0.0025(9) 0.0016(9) -0.0057(10) C59 0.0172(12) 0.0181(11) 0.0157(11) -0.0026(8) 0.0015(8) -0.0063(8) C60 0.0173(12) 0.0155(11) 0.0167(11) -0.0032(8) 0.0036(8) -0.0073(8) C61 0.0213(13) 0.0272(13) 0.0191(12) -0.0070(9) 0.0044(9) -0.0066(9) C62 0.0195(13) 0.0264(13) 0.0265(13) -0.0143(10) 0.0097(9) -0.0077(9) C63 0.0154(12) 0.0193(12) 0.0308(13) -0.0046(10) 0.0065(9) -0.0037(8) C64 0.0195(12) 0.0171(11) 0.0195(11) -0.0001(9) 0.0039(8) -0.0004(8) O5W 0.0190(9) 0.0185(9) 0.0344(10) -0.0050(7) 0.0015(7) 0.0026(6) _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 O2 2.1014(15) . ? Mn1 O8 2.1127(15) 2_645 ? Mn1 O2W 2.2190(16) . ? Mn1 O1W 2.2296(16) . ? Mn1 N1 2.2315(18) . ? Mn1 N2 2.2761(19) . ? Mn2 O7 2.1625(15) 2_645 ? Mn2 O3W 2.1636(15) . ? Mn2 O1 2.1675(15) . ? Mn2 O4W 2.2504(16) . ? Mn2 N3 2.2628(18) . ? Mn2 N4 2.2929(18) . ? Mn3 O14 2.1152(15) . ? Mn3 O20 2.1207(15) 2_545 ? Mn3 O6W 2.1898(16) . ? Mn3 O5W 2.2372(17) . ? Mn3 N5 2.2464(19) . ? Mn3 N6 2.2611(18) . ? Mn4 O13 2.1462(15) . ? Mn4 O19 2.1720(14) 2_545 ? Mn4 O7W 2.1819(15) . ? Mn4 O8W 2.2339(16) . ? Mn4 N8 2.2724(18) . ? Mn4 N7 2.2817(18) . ? O1 C1 1.248(3) . ? O2 C1 1.251(3) . ? O3 C2 1.214(3) . ? O4 C2 1.313(2) . ? O5 C3 1.231(3) . ? O6 C3 1.287(3) . ? O7 C4 1.254(2) . ? O7 Mn2 2.1624(15) 2_655 ? O8 C4 1.255(3) . ? O8 Mn1 2.1127(15) 2_655 ? O9 C5 1.285(3) . ? O10 C5 1.231(3) . ? O11 C6 1.286(3) . ? O12 C6 1.228(3) . ? O13 C13 1.244(3) . ? O14 C13 1.254(3) . ? O15 C14 1.295(3) . ? O16 C14 1.223(3) . ? O17 C15 1.280(3) . ? O18 C15 1.233(3) . ? O19 C16 1.248(2) . ? O19 Mn4 2.1720(14) 2 ? O20 C16 1.261(2) . ? O20 Mn3 2.1208(15) 2 ? O21 C17 1.290(2) . ? O22 C17 1.227(3) . ? O23 C18 1.309(2) . ? O24 C18 1.216(3) . ? N1 C25 1.337(3) . ? N1 C29 1.351(3) . ? N2 C34 1.341(3) . ? N2 C30 1.350(3) . ? N3 C35 1.343(3) . ? N3 C39 1.345(3) . ? N4 C44 1.343(3) . ? N4 C40 1.352(3) . ? N5 C45 1.339(3) . ? N5 C49 1.344(3) . ? N6 C54 1.338(3) . ? N6 C50 1.352(3) . ? N7 C55 1.341(3) . ? N7 C59 1.349(3) . ? N8 C64 1.342(3) . ? N8 C60 1.344(3) . ? C1 C7 1.513(3) . ? C2 C8 1.508(3) . ? C3 C9 1.516(3) . ? C4 C10 1.518(3) . ? C5 C11 1.511(3) . ? C6 C12 1.514(3) . ? C7 C12 1.399(3) . ? C7 C8 1.404(3) . ? C8 C9 1.394(3) . ? C9 C10 1.400(3) . ? C10 C11 1.398(3) . ? C11 C12 1.395(3) . ? C13 C19 1.519(3) . ? C14 C20 1.511(3) . ? C15 C21 1.521(3) . ? C16 C22 1.515(3) . ? C17 C23 1.512(3) . ? C18 C24 1.508(3) . ? C19 C24 1.389(3) . ? C19 C20 1.397(3) . ? C20 C21 1.398(3) . ? C21 C22 1.404(3) . ? C22 C23 1.408(3) . ? C23 C24 1.392(3) . ? C25 C26 1.385(3) . ? C26 C27 1.384(4) . ? C27 C28 1.385(4) . ? C28 C29 1.387(3) . ? C29 C30 1.483(3) . ? C30 C31 1.396(3) . ? C31 C32 1.381(4) . ? C32 C33 1.384(4) . ? C33 C34 1.383(3) . ? C35 C36 1.385(3) . ? C36 C37 1.380(3) . ? C37 C38 1.389(3) . ? C38 C39 1.393(3) . ? C39 C40 1.482(3) . ? C40 C41 1.391(3) . ? C41 C42 1.384(3) . ? C42 C43 1.381(4) . ? C43 C44 1.388(3) . ? C45 C46 1.389(3) . ? C46 C47 1.374(4) . ? C47 C48 1.385(4) . ? C48 C49 1.393(3) . ? C49 C50 1.490(3) . ? C50 C51 1.390(3) . ? C51 C52 1.383(4) . ? C52 C53 1.378(4) . ? C53 C54 1.383(3) . ? C55 C56 1.385(3) . ? C56 C57 1.380(4) . ? C57 C58 1.382(4) . ? C58 C59 1.395(3) . ? C59 C60 1.486(3) . ? C60 C61 1.393(3) . ? C61 C62 1.386(4) . ? C62 C63 1.382(3) . ? C63 C64 1.386(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 O2 Mn1 O8 109.34(6) . 2_645 ? O2 Mn1 O2W 90.63(6) . . ? O8 Mn1 O2W 85.71(6) 2_645 . ? O2 Mn1 O1W 89.58(6) . . ? O8 Mn1 O1W 87.56(6) 2_645 . ? O2W Mn1 O1W 172.93(6) . . ? O2 Mn1 N1 156.76(7) . . ? O8 Mn1 N1 92.50(7) 2_645 . ? O2W Mn1 N1 99.10(6) . . ? O1W Mn1 N1 83.32(6) . . ? O2 Mn1 N2 86.72(6) . . ? O8 Mn1 N2 162.11(7) 2_645 . ? O2W Mn1 N2 86.30(6) . . ? O1W Mn1 N2 100.76(6) . . ? N1 Mn1 N2 73.01(7) . . ? O7 Mn2 O3W 83.86(6) 2_645 . ? O7 Mn2 O1 134.03(6) 2_645 . ? O3W Mn2 O1 86.05(6) . . ? O7 Mn2 O4W 80.52(6) 2_645 . ? O3W Mn2 O4W 144.97(6) . . ? O1 Mn2 O4W 82.70(6) . . ? O7 Mn2 N3 138.25(6) 2_645 . ? O3W Mn2 N3 83.38(6) . . ? O1 Mn2 N3 84.34(6) . . ? O4W Mn2 N3 127.99(6) . . ? O7 Mn2 N4 82.94(6) 2_645 . ? O3W Mn2 N4 122.21(7) . . ? O1 Mn2 N4 138.31(6) . . ? O4W Mn2 N4 86.74(6) . . ? N3 Mn2 N4 70.95(7) . . ? O14 Mn3 O20 113.50(6) . 2_545 ? O14 Mn3 O6W 90.26(6) . . ? O20 Mn3 O6W 88.29(6) 2_545 . ? O14 Mn3 O5W 83.67(6) . . ? O20 Mn3 O5W 88.71(6) 2_545 . ? O6W Mn3 O5W 171.52(7) . . ? O14 Mn3 N5 152.82(7) . . ? O20 Mn3 N5 89.56(6) 2_545 . ? O6W Mn3 N5 105.27(7) . . ? O5W Mn3 N5 82.63(7) . . ? O14 Mn3 N6 88.08(6) . . ? O20 Mn3 N6 156.26(6) 2_545 . ? O6W Mn3 N6 81.57(6) . . ? O5W Mn3 N6 104.06(7) . . ? N5 Mn3 N6 72.71(7) . . ? O13 Mn4 O19 132.93(6) . 2_545 ? O13 Mn4 O7W 87.24(6) . . ? O19 Mn4 O7W 82.58(6) 2_545 . ? O13 Mn4 O8W 85.43(6) . . ? O19 Mn4 O8W 79.86(6) 2_545 . ? O7W Mn4 O8W 147.98(6) . . ? O13 Mn4 N8 81.68(6) . . ? O19 Mn4 N8 142.25(6) 2_545 . ? O7W Mn4 N8 85.23(6) . . ? O8W Mn4 N8 124.25(6) . . ? O13 Mn4 N7 139.28(6) . . ? O19 Mn4 N7 83.89(6) 2_545 . ? O7W Mn4 N7 119.14(6) . . ? O8W Mn4 N7 85.37(6) . . ? N8 Mn4 N7 71.28(7) . . ? C1 O1 Mn2 133.22(14) . . ? C1 O2 Mn1 139.70(14) . . ? C4 O7 Mn2 122.73(13) . 2_655 ? C4 O8 Mn1 152.82(14) . 2_655 ? C13 O13 Mn4 137.72(14) . . ? C13 O14 Mn3 137.45(14) . . ? C16 O19 Mn4 121.69(13) . 2 ? C16 O20 Mn3 150.49(14) . 2 ? C25 N1 C29 118.7(2) . . ? C25 N1 Mn1 122.41(15) . . ? C29 N1 Mn1 116.99(15) . . ? C34 N2 C30 118.4(2) . . ? C34 N2 Mn1 124.59(16) . . ? C30 N2 Mn1 116.09(15) . . ? C35 N3 C39 118.98(19) . . ? C35 N3 Mn2 121.32(14) . . ? C39 N3 Mn2 119.57(14) . . ? C44 N4 C40 118.27(19) . . ? C44 N4 Mn2 123.30(15) . . ? C40 N4 Mn2 118.35(14) . . ? C45 N5 C49 118.6(2) . . ? C45 N5 Mn3 122.53(15) . . ? C49 N5 Mn3 117.50(15) . . ? C54 N6 C50 118.6(2) . . ? C54 N6 Mn3 123.15(15) . . ? C50 N6 Mn3 116.89(15) . . ? C55 N7 C59 118.17(19) . . ? C55 N7 Mn4 123.39(15) . . ? C59 N7 Mn4 118.25(15) . . ? C64 N8 C60 118.85(19) . . ? C64 N8 Mn4 122.23(15) . . ? C60 N8 Mn4 118.80(15) . . ? O1 C1 O2 127.5(2) . . ? O1 C1 C7 116.17(18) . . ? O2 C1 C7 116.35(18) . . ? O3 C2 O4 125.05(19) . . ? O3 C2 C8 122.29(18) . . ? O4 C2 C8 112.59(17) . . ? O5 C3 O6 125.34(19) . . ? O5 C3 C9 118.54(18) . . ? O6 C3 C9 116.11(18) . . ? O7 C4 O8 126.25(19) . . ? O7 C4 C10 117.19(18) . . ? O8 C4 C10 116.38(18) . . ? O10 C5 O9 125.86(19) . . ? O10 C5 C11 119.35(18) . . ? O9 C5 C11 114.78(17) . . ? O12 C6 O11 125.50(19) . . ? O12 C6 C12 118.79(19) . . ? O11 C6 C12 115.70(17) . . ? C12 C7 C8 119.37(18) . . ? C12 C7 C1 120.21(18) . . ? C8 C7 C1 120.43(17) . . ? C9 C8 C7 121.11(18) . . ? C9 C8 C2 121.20(18) . . ? C7 C8 C2 117.68(18) . . ? C8 C9 C10 119.11(18) . . ? C8 C9 C3 119.33(18) . . ? C10 C9 C3 121.50(18) . . ? C11 C10 C9 119.87(18) . . ? C11 C10 C4 117.51(17) . . ? C9 C10 C4 122.60(18) . . ? C12 C11 C10 120.77(18) . . ? C12 C11 C5 118.59(18) . . ? C10 C11 C5 120.63(18) . . ? C11 C12 C7 119.51(18) . . ? C11 C12 C6 119.05(18) . . ? C7 C12 C6 121.40(18) . . ? O13 C13 O14 127.6(2) . . ? O13 C13 C19 117.20(18) . . ? O14 C13 C19 115.16(18) . . ? O16 C14 O15 125.66(19) . . ? O16 C14 C20 120.25(19) . . ? O15 C14 C20 114.07(17) . . ? O18 C15 O17 125.20(19) . . ? O18 C15 C21 117.43(18) . . ? O17 C15 C21 117.35(17) . . ? O19 C16 O20 126.03(19) . . ? O19 C16 C22 117.59(18) . . ? O20 C16 C22 116.37(18) . . ? O22 C17 O21 126.15(19) . . ? O22 C17 C23 119.68(18) . . ? O21 C17 C23 114.16(17) . . ? O24 C18 O23 125.30(19) . . ? O24 C18 C24 121.96(18) . . ? O23 C18 C24 112.71(17) . . ? C24 C19 C20 119.72(18) . . ? C24 C19 C13 118.32(17) . . ? C20 C19 C13 121.94(17) . . ? C19 C20 C21 120.31(18) . . ? C19 C20 C14 118.99(18) . . ? C21 C20 C14 120.68(18) . . ? C20 C21 C22 119.78(18) . . ? C20 C21 C15 118.60(17) . . ? C22 C21 C15 121.45(18) . . ? C21 C22 C23 119.33(18) . . ? C21 C22 C16 120.92(18) . . ? C23 C22 C16 119.75(17) . . ? C24 C23 C22 119.99(18) . . ? C24 C23 C17 117.66(18) . . ? C22 C23 C17 122.34(18) . . ? C19 C24 C23 120.52(18) . . ? C19 C24 C18 118.25(18) . . ? C23 C24 C18 121.21(17) . . ? N1 C25 C26 122.7(2) . . ? C27 C26 C25 118.5(2) . . ? C26 C27 C28 119.4(2) . . ? C27 C28 C29 118.9(2) . . ? N1 C29 C28 121.8(2) . . ? N1 C29 C30 115.8(2) . . ? C28 C29 C30 122.4(2) . . ? N2 C30 C31 121.5(2) . . ? N2 C30 C29 115.62(19) . . ? C31 C30 C29 122.9(2) . . ? C32 C31 C30 119.4(2) . . ? C31 C32 C33 119.1(2) . . ? C34 C33 C32 118.6(3) . . ? N2 C34 C33 123.1(2) . . ? N3 C35 C36 122.7(2) . . ? C37 C36 C35 118.5(2) . . ? C36 C37 C38 119.3(2) . . ? C37 C38 C39 119.2(2) . . ? N3 C39 C38 121.4(2) . . ? N3 C39 C40 115.57(19) . . ? C38 C39 C40 123.1(2) . . ? N4 C40 C41 121.7(2) . . ? N4 C40 C39 115.41(19) . . ? C41 C40 C39 122.8(2) . . ? C42 C41 C40 119.3(2) . . ? C43 C42 C41 119.1(2) . . ? C42 C43 C44 118.6(2) . . ? N4 C44 C43 123.0(2) . . ? N5 C45 C46 122.8(2) . . ? C47 C46 C45 118.4(2) . . ? C46 C47 C48 119.6(2) . . ? C47 C48 C49 118.8(2) . . ? N5 C49 C48 121.8(2) . . ? N5 C49 C50 115.6(2) . . ? C48 C49 C50 122.6(2) . . ? N6 C50 C51 121.5(2) . . ? N6 C50 C49 115.35(19) . . ? C51 C50 C49 123.1(2) . . ? C52 C51 C50 119.0(2) . . ? C53 C52 C51 119.6(2) . . ? C52 C53 C54 118.4(2) . . ? N6 C54 C53 122.9(2) . . ? N7 C55 C56 123.2(2) . . ? C57 C56 C55 118.5(2) . . ? C56 C57 C58 119.2(2) . . ? C57 C58 C59 119.2(2) . . ? N7 C59 C58 121.7(2) . . ? N7 C59 C60 115.44(19) . . ? C58 C59 C60 122.9(2) . . ? N8 C60 C61 121.7(2) . . ? N8 C60 C59 115.64(19) . . ? C61 C60 C59 122.6(2) . . ? C62 C61 C60 119.0(2) . . ? C63 C62 C61 119.2(2) . . ? C62 C63 C64 118.7(2) . . ? N8 C64 C63 122.5(2) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 71.41 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.685 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.056 data_twin5z _database_code_depnum_ccdc_archive 'CCDC 903330' #TrackingRef 'web_deposit_cif_file_0_SlaviSevov_1349089406.5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Mn2(H2mel)(phen)2(H2O)2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H44 Mn4 N8 O28' _chemical_formula_weight 1688.91 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' 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 9.0764(3) _cell_length_b 21.9597(8) _cell_length_c 16.5364(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.617(2) _cell_angle_gamma 90.00 _cell_volume 3285.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 2619 _cell_measurement_theta_min 4.03 _cell_measurement_theta_max 70.36 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.043 _exptl_crystal_size_min 0.031 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 6.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 0.753 _exptl_absorpt_process_details 'Blessing, R.H. (1995) Acta Cryst. A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6167 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 71.34 _reflns_number_total 6167 _reflns_number_gt 5429 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0474P)^2^+6.6520P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6167 _refine_ls_number_parameters 753 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.74947(6) 0.15811(2) 0.91424(3) 0.01662(12) Uani 1 1 d . . . Mn2 Mn 0.71943(6) 0.33374(2) 0.90906(3) 0.01687(12) Uani 1 1 d . . . O1 O 0.5986(3) 0.19568(12) 1.00049(15) 0.0298(6) Uani 1 1 d . A . O2 O 0.5421(3) 0.28951(13) 0.95569(15) 0.0330(6) Uani 1 1 d . A . O3 O 0.2864(3) 0.20603(12) 0.87371(14) 0.0305(6) Uani 1 1 d . . . O4 O 0.1703(3) 0.29526(11) 0.87862(14) 0.0313(6) Uani 1 1 d . . . H4 H 0.1463 0.2884 0.8294 0.047 Uiso 1 1 calc R . . O5 O -0.0636(2) 0.20448(10) 0.96479(14) 0.0248(5) Uani 1 1 d . . . O6 O -0.1032(3) 0.30312(11) 0.98858(15) 0.0276(6) Uani 1 1 d . . . O9 O 0.2252(3) 0.20703(16) 1.29538(16) 0.0487(9) Uani 1 1 d . . . O10 O 0.3013(3) 0.30360(13) 1.29737(16) 0.0397(7) Uani 1 1 d . . . O11 O 0.5546(3) 0.20545(12) 1.23606(15) 0.0302(6) Uani 1 1 d . . . O12 O 0.6434(3) 0.27483(15) 1.15421(17) 0.0389(7) Uani 1 1 d . . . H12 H 0.7264 0.2608 1.1709 0.058 Uiso 1 1 calc R . . C25 C 0.3872(4) 0.24604(13) 1.0456(2) 0.0169(7) Uani 1 1 d . A . C26 C 0.2497(4) 0.25072(13) 1.0022(2) 0.0168(7) Uani 1 1 d . . . C27 C 0.1203(3) 0.25654(12) 1.0421(2) 0.0157(6) Uani 1 1 d . . . C28 C 0.1297(4) 0.25851(15) 1.1267(2) 0.0191(7) Uani 1 1 d . C . C29 C 0.2662(4) 0.25269(14) 1.1709(2) 0.0194(7) Uani 1 1 d . . . C30 C 0.3959(3) 0.24624(13) 1.1305(2) 0.0174(6) Uani 1 1 d . . . C31 C 0.5235(4) 0.24306(16) 0.9977(2) 0.0212(7) Uani 1 1 d . . . C32 C 0.2390(4) 0.24802(14) 0.9110(2) 0.0190(7) Uani 1 1 d . . . C33 C -0.0290(3) 0.25533(13) 0.9941(2) 0.0167(6) Uani 1 1 d . . . C34 C -0.0109(5) 0.2715(2) 1.1676(2) 0.0399(10) Uani 1 1 d . . . C35 C 0.2674(4) 0.25455(17) 1.2629(2) 0.0260(8) Uani 1 1 d . . . C36 C 0.5429(4) 0.24111(15) 1.1781(2) 0.0211(6) Uani 1 1 d . . . N1A N 0.7652(7) 0.0876(3) 1.0185(4) 0.0231(12) Uani 0.50 1 d P A 1 N2A N 0.8265(7) 0.0660(3) 0.8642(4) 0.0244(12) Uani 0.50 1 d P A 1 C1A C 0.7399(9) 0.0997(4) 1.0952(4) 0.0338(17) Uani 0.50 1 d P A 1 H1AA H 0.7219 0.1406 1.1107 0.041 Uiso 0.50 1 calc PR A 1 C2A C 0.7395(10) 0.0531(4) 1.1537(5) 0.043(2) Uani 0.50 1 d P A 1 H2AA H 0.7239 0.0631 1.2082 0.052 Uiso 0.50 1 calc PR A 1 C3A C 0.7607(10) -0.0051(4) 1.1338(6) 0.045(2) Uani 0.50 1 d P A 1 H3AA H 0.7561 -0.0363 1.1733 0.054 Uiso 0.50 1 calc PR A 1 C4A C 0.7899(9) -0.0196(4) 1.0534(6) 0.0362(19) Uani 0.50 1 d P A 1 C5A C 0.7913(8) 0.0293(3) 0.9976(7) 0.0236(15) Uani 0.50 1 d P A 1 C6A C 0.8173(10) -0.0802(4) 1.0271(7) 0.049(2) Uani 0.50 1 d P A 1 H6AA H 0.8136 -0.1134 1.0636 0.059 Uiso 0.50 1 calc PR A 1 C7A C 0.8508(6) -0.09016(18) 0.9444(4) 0.0531(13) Uani 0.50 1 d P A 1 H7AA H 0.8767 -0.1298 0.9273 0.064 Uiso 0.50 1 calc PR A 1 C8A C 0.8456(9) -0.0431(4) 0.8906(6) 0.0367(19) Uani 0.50 1 d P A 1 C9A C 0.8227(11) 0.0170(5) 0.9153(8) 0.019(2) Uani 0.50 1 d P A 1 C10A C 0.8741(9) -0.0526(4) 0.8098(6) 0.044(2) Uani 0.50 1 d P A 1 H10A H 0.8891 -0.0927 0.7905 0.052 Uiso 0.50 1 calc PR A 1 C11A C 0.8802(9) -0.0047(4) 0.7593(5) 0.040(2) Uani 0.50 1 d P A 1 H11A H 0.9002 -0.0108 0.7044 0.048 Uiso 0.50 1 calc PR A 1 C12A C 0.8564(8) 0.0553(4) 0.7889(5) 0.0323(17) Uani 0.50 1 d P A 1 H12A H 0.8623 0.0887 0.7529 0.039 Uiso 0.50 1 calc PR A 1 N3A N 0.8489(11) 0.4174(5) 0.8733(6) 0.0229(18) Uani 0.50 1 d P B 1 N4A N 0.6588(10) 0.4113(6) 0.9895(8) 0.019(2) Uani 0.50 1 d P B 1 C13A C 0.9386(9) 0.4189(4) 0.8146(5) 0.0339(17) Uani 0.50 1 d P B 1 H13A H 0.9502 0.3833 0.7830 0.041 Uiso 0.50 1 calc PR B 1 C14A C 1.0182(9) 0.4719(4) 0.7972(6) 0.041(2) Uani 0.50 1 d P B 1 H14A H 1.0842 0.4713 0.7554 0.049 Uiso 0.50 1 calc PR B 1 C15A C 1.0002(10) 0.5241(4) 0.8405(6) 0.042(2) Uani 0.50 1 d P B 1 H15A H 1.0519 0.5602 0.8286 0.051 Uiso 0.50 1 calc PR B 1 C16A C 0.9035(13) 0.5233(5) 0.9031(7) 0.037(2) Uani 0.50 1 d P B 1 C17A C 0.826(3) 0.4667(9) 0.9179(8) 0.025(4) Uani 0.50 1 d P B 1 C18A C 0.873(2) 0.5736(8) 0.9525(9) 0.042(5) Uani 0.50 1 d P B 1 H18A H 0.9261 0.6103 0.9454 0.050 Uiso 0.50 1 calc PR B 1 C19A C 0.7752(17) 0.5728(8) 1.0089(14) 0.052(4) Uani 0.50 1 d P B 1 H19A H 0.7557 0.6089 1.0379 0.063 Uiso 0.50 1 calc PR B 1 C20A C 0.7004(12) 0.5178(4) 1.0249(6) 0.034(2) Uani 0.50 1 d P B 1 C21A C 0.7271(11) 0.4649(4) 0.9815(5) 0.022(2) Uiso 0.50 1 d P B 1 C22A C 0.5998(10) 0.5128(4) 1.0848(5) 0.040(2) Uani 0.50 1 d P B 1 H22A H 0.5783 0.5471 1.1170 0.048 Uiso 0.50 1 calc PR B 1 C23A C 0.5341(9) 0.4585(4) 1.0962(5) 0.0368(18) Uani 0.50 1 d P B 1 H23A H 0.4654 0.4545 1.1363 0.044 Uiso 0.50 1 calc PR B 1 C24A C 0.5671(10) 0.4083(3) 1.0491(4) 0.0282(16) Uani 0.50 1 d P B 1 H24A H 0.5226 0.3703 1.0598 0.034 Uiso 0.50 1 calc PR B 1 O7B O -0.1014(4) 0.22933(18) 1.1666(2) 0.0593(10) Uani 1 1 d . C 1 O8B O -0.0267(4) 0.32348(16) 1.19688(19) 0.0505(8) Uani 1 1 d . C 1 N1B N 0.7087(7) 0.0659(3) 0.9722(4) 0.0257(13) Uani 0.50 1 d P A 2 N2B N 0.9161(7) 0.0912(3) 0.8684(4) 0.0234(12) Uani 0.50 1 d P A 2 C1B C 0.6067(8) 0.0536(4) 1.0221(5) 0.0346(18) Uani 0.50 1 d P A 2 H1BA H 0.5511 0.0863 1.0418 0.042 Uiso 0.50 1 calc PR A 2 C2B C 0.5767(9) -0.0057(4) 1.0475(5) 0.043(2) Uani 0.50 1 d P . 2 H2BA H 0.5009 -0.0128 1.0827 0.052 Uiso 0.50 1 calc PR . 2 C3B C 0.6570(11) -0.0530(4) 1.0212(5) 0.044(2) Uani 0.50 1 d P A 2 H3BA H 0.6376 -0.0935 1.0377 0.052 Uiso 0.50 1 calc PR A 2 C4B C 0.7689(10) -0.0414(3) 0.9695(5) 0.0359(19) Uani 0.50 1 d P A 2 C5B C 0.7902(15) 0.0187(5) 0.9462(7) 0.022(2) Uani 0.50 1 d P A 2 C6B C 0.8508(6) -0.09016(18) 0.9444(4) 0.0531(13) Uani 0.50 1 d P A 2 H6BA H 0.8320 -0.1307 0.9609 0.064 Uiso 0.50 1 calc PR A 2 C7B C 0.9666(11) -0.0765(4) 0.8916(6) 0.048(2) Uani 0.50 1 d P A 2 H7BA H 1.0272 -0.1084 0.8743 0.057 Uiso 0.50 1 calc PR A 2 C8B C 0.9912(9) -0.0149(4) 0.8650(5) 0.0338(17) Uani 0.50 1 d P A 2 C9B C 0.9019(10) 0.0321(4) 0.8914(5) 0.0245(15) Uani 0.50 1 d P A 2 C10B C 1.1018(10) 0.0013(4) 0.8148(5) 0.044(2) Uani 0.50 1 d P A 2 H10B H 1.1642 -0.0290 0.7948 0.053 Uiso 0.50 1 calc PR A 2 C11B C 1.1194(9) 0.0615(5) 0.7946(5) 0.044(2) Uani 0.50 1 d P A 2 H11B H 1.1965 0.0733 0.7623 0.053 Uiso 0.50 1 calc PR A 2 C12B C 1.0239(8) 0.1047(4) 0.8217(5) 0.0335(17) Uani 0.50 1 d P A 2 H12B H 1.0361 0.1459 0.8062 0.040 Uiso 0.50 1 calc PR A 2 N3B N 0.8039(11) 0.4144(4) 0.8456(5) 0.0218(18) Uani 0.50 1 d P B 2 N4B N 0.7123(11) 0.4115(6) 0.9970(8) 0.023(2) Uani 0.50 1 d P B 2 C13B C 0.8443(9) 0.4159(4) 0.7692(5) 0.0334(17) Uani 0.50 1 d P B 2 H13B H 0.8339 0.3801 0.7370 0.040 Uiso 0.50 1 calc PR B 2 C14B C 0.9009(10) 0.4683(5) 0.7357(6) 0.047(2) Uani 0.50 1 d P B 2 H14B H 0.9287 0.4675 0.6816 0.057 Uiso 0.50 1 calc PR B 2 C15B C 0.9167(11) 0.5202(4) 0.7796(8) 0.057(3) Uani 0.50 1 d P B 2 H15B H 0.9540 0.5560 0.7561 0.069 Uiso 0.50 1 calc PR B 2 C16B C 0.8766(13) 0.5211(4) 0.8623(8) 0.041(3) Uani 0.50 1 d P B 2 C17B C 0.820(2) 0.4678(11) 0.8898(10) 0.026(4) Uani 0.50 1 d P B 2 C18B C 0.892(2) 0.5752(8) 0.9139(11) 0.056(5) Uani 0.50 1 d P B 2 H18B H 0.9321 0.6119 0.8948 0.067 Uiso 0.50 1 calc PR B 2 C19B C 0.846(3) 0.5711(8) 0.9902(15) 0.053(8) Uani 0.50 1 d P B 2 H19B H 0.8548 0.6058 1.0247 0.063 Uiso 0.50 1 calc PR B 2 C20B C 0.7847(14) 0.5167(4) 1.0199(7) 0.044(3) Uani 0.50 1 d P B 2 C21B C 0.7694(11) 0.4653(4) 0.9686(6) 0.0215(19) Uiso 0.50 1 d P B 2 C22B C 0.7368(13) 0.5131(5) 1.0965(6) 0.059(3) Uani 0.50 1 d P B 2 H22B H 0.7442 0.5475 1.1315 0.070 Uiso 0.50 1 calc PR B 2 C23B C 0.6781(12) 0.4597(5) 1.1222(6) 0.057(3) Uani 0.50 1 d P B 2 H23B H 0.6441 0.4566 1.1749 0.068 Uiso 0.50 1 calc PR B 2 C24B C 0.6689(12) 0.4095(4) 1.0695(5) 0.040(2) Uani 0.50 1 d P B 2 H24B H 0.6291 0.3725 1.0879 0.048 Uiso 0.50 1 calc PR B 2 O1W O 0.5344(3) 0.13704(12) 0.84781(16) 0.0284(5) Uani 1 1 d D A . H1W H 0.529(5) 0.145(2) 0.7984(9) 0.043 Uiso 1 1 d D . . H2W H 0.463(3) 0.1551(19) 0.865(3) 0.043 Uiso 1 1 d D . . O2W O 0.4702(4) 0.36459(17) 0.8221(3) 0.0637(10) Uani 1 1 d D . . H3W H 0.387(4) 0.364(3) 0.796(4) 0.096 Uiso 1 1 d D . . H4W H 0.477(8) 0.342(3) 0.781(3) 0.096 Uiso 1 1 d 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 0.0150(3) 0.0165(2) 0.0184(3) -0.00045(19) 0.00116(18) -0.00077(17) Mn2 0.0168(3) 0.0170(2) 0.0171(2) 0.00031(19) 0.00328(18) -0.00031(18) O1 0.0191(13) 0.0449(15) 0.0260(13) -0.0068(11) 0.0047(10) 0.0061(11) O2 0.0162(13) 0.0550(17) 0.0278(13) 0.0149(12) 0.0016(10) -0.0087(11) O3 0.0261(14) 0.0462(15) 0.0192(12) -0.0093(11) 0.0008(10) 0.0128(11) O4 0.0464(17) 0.0328(14) 0.0132(11) 0.0004(10) -0.0066(10) 0.0112(11) O5 0.0190(12) 0.0250(12) 0.0292(13) -0.0044(10) -0.0044(9) -0.0046(9) O6 0.0199(13) 0.0262(12) 0.0349(14) -0.0025(10) -0.0085(10) 0.0063(9) O9 0.0494(19) 0.077(2) 0.0194(13) 0.0138(14) -0.0006(12) -0.0305(16) O10 0.0532(19) 0.0468(17) 0.0193(12) -0.0057(12) 0.0046(12) 0.0181(14) O11 0.0268(14) 0.0396(14) 0.0225(12) 0.0088(11) -0.0083(10) -0.0027(11) O12 0.0132(13) 0.067(2) 0.0361(15) 0.0181(14) -0.0024(11) -0.0083(12) C25 0.0138(18) 0.0195(16) 0.0176(16) 0.0002(11) 0.0022(13) -0.0019(11) C26 0.0153(18) 0.0194(16) 0.0157(16) -0.0006(11) 0.0006(13) -0.0014(10) C27 0.0152(17) 0.0140(13) 0.0176(16) -0.0004(11) -0.0008(12) -0.0010(10) C28 0.0171(18) 0.0223(15) 0.0178(16) 0.0032(12) 0.0001(13) -0.0012(12) C29 0.0170(19) 0.0252(17) 0.0160(16) 0.0027(12) 0.0017(13) -0.0015(11) C30 0.0134(17) 0.0210(15) 0.0180(16) 0.0012(11) 0.0016(12) 0.0000(11) C31 0.0147(18) 0.0371(19) 0.0113(15) -0.0033(13) -0.0017(12) -0.0034(13) C32 0.0122(17) 0.0280(18) 0.0163(16) -0.0017(12) -0.0011(12) -0.0045(11) C33 0.0135(17) 0.0228(15) 0.0141(15) 0.0014(11) 0.0021(12) -0.0017(11) C34 0.031(2) 0.075(3) 0.0131(17) 0.0032(19) -0.0019(15) -0.011(2) C35 0.0074(18) 0.053(2) 0.0172(17) 0.0040(15) 0.0003(13) 0.0040(13) C36 0.0165(17) 0.0286(16) 0.0184(16) -0.0042(13) 0.0024(12) 0.0017(12) N1A 0.022(3) 0.023(3) 0.024(3) 0.004(2) 0.001(2) -0.004(2) N2A 0.026(4) 0.024(3) 0.023(3) -0.001(2) 0.003(3) 0.003(3) C1A 0.031(4) 0.046(5) 0.024(4) 0.006(3) 0.001(3) -0.005(3) C2A 0.035(5) 0.064(6) 0.029(4) 0.014(4) -0.001(3) -0.007(4) C3A 0.034(5) 0.056(6) 0.042(5) 0.028(4) -0.007(4) -0.006(4) C4A 0.025(4) 0.030(4) 0.052(5) 0.016(4) -0.004(3) -0.006(3) C5A 0.012(4) 0.022(4) 0.036(5) 0.009(4) -0.001(3) -0.001(3) C6A 0.046(6) 0.023(4) 0.077(7) 0.023(4) -0.008(5) -0.002(4) C7A 0.063(3) 0.0183(18) 0.074(4) 0.000(2) -0.016(3) 0.0035(19) C8A 0.021(4) 0.026(4) 0.061(6) -0.007(4) -0.007(4) 0.006(3) C9A 0.011(6) 0.020(4) 0.027(7) -0.001(5) -0.004(4) 0.004(4) C10A 0.032(5) 0.030(4) 0.067(6) -0.023(4) -0.006(4) 0.007(3) C11A 0.031(5) 0.049(5) 0.040(5) -0.020(4) 0.001(3) 0.001(4) C12A 0.028(4) 0.038(4) 0.030(4) -0.005(3) -0.003(3) 0.004(3) N3A 0.014(5) 0.026(4) 0.028(5) 0.004(4) -0.001(3) -0.002(3) N4A 0.009(6) 0.022(3) 0.023(4) 0.001(3) -0.009(5) 0.006(4) C13A 0.036(5) 0.030(4) 0.037(4) 0.009(3) 0.007(4) 0.006(3) C14A 0.025(4) 0.044(5) 0.054(5) 0.015(4) 0.011(4) -0.004(3) C15A 0.030(5) 0.038(5) 0.057(6) 0.017(4) -0.002(4) -0.008(3) C16A 0.026(6) 0.037(6) 0.045(6) 0.008(5) -0.008(5) -0.008(4) C17A 0.032(6) 0.009(4) 0.033(9) 0.010(6) -0.004(8) -0.004(3) C18A 0.051(11) 0.022(6) 0.051(12) 0.013(11) -0.004(12) -0.013(5) C19A 0.062(11) 0.030(6) 0.062(9) -0.013(5) -0.013(10) 0.000(8) C20A 0.032(5) 0.029(4) 0.040(5) -0.008(3) -0.006(5) 0.008(4) C22A 0.041(5) 0.038(4) 0.038(5) -0.018(4) -0.011(4) 0.016(4) C23A 0.032(5) 0.047(5) 0.031(4) -0.008(3) 0.001(3) 0.014(4) C24A 0.029(5) 0.032(4) 0.023(4) -0.002(3) 0.005(3) 0.008(3) O7B 0.045(2) 0.081(3) 0.056(2) -0.0182(19) 0.0224(16) -0.0252(18) O8B 0.0469(19) 0.065(2) 0.0406(17) -0.0050(16) 0.0107(14) 0.0208(16) N1B 0.020(3) 0.021(3) 0.037(4) 0.002(3) 0.004(3) 0.001(2) N2B 0.019(3) 0.024(3) 0.028(3) -0.003(2) 0.004(2) -0.004(3) C1B 0.023(4) 0.038(4) 0.043(5) 0.015(3) 0.002(3) 0.002(3) C2B 0.031(5) 0.053(5) 0.044(5) 0.022(4) -0.003(3) -0.019(4) C3B 0.056(6) 0.027(4) 0.046(5) 0.019(4) -0.009(4) -0.015(4) C4B 0.044(5) 0.026(4) 0.035(4) 0.009(3) -0.014(4) -0.002(3) C5B 0.023(6) 0.016(4) 0.025(7) -0.003(5) 0.001(5) 0.001(3) C6B 0.063(3) 0.0183(18) 0.074(4) 0.000(2) -0.016(3) 0.0035(19) C7B 0.059(6) 0.030(4) 0.051(6) -0.011(4) -0.017(5) 0.016(4) C8B 0.034(4) 0.031(4) 0.034(4) -0.012(3) -0.009(3) 0.010(3) C9B 0.021(4) 0.025(4) 0.027(4) -0.006(3) -0.002(4) 0.001(3) C10B 0.036(5) 0.055(5) 0.041(5) -0.019(4) 0.001(4) 0.021(4) C11B 0.030(5) 0.071(6) 0.034(4) -0.014(4) 0.011(3) 0.006(4) C12B 0.026(4) 0.042(4) 0.033(4) -0.005(3) 0.005(3) -0.003(3) N3B 0.020(6) 0.018(3) 0.027(5) -0.001(3) 0.001(3) 0.000(3) N4B 0.014(7) 0.034(4) 0.020(4) -0.006(3) -0.011(5) 0.008(5) C13B 0.029(4) 0.042(4) 0.030(4) 0.015(3) 0.002(3) 0.003(3) C14B 0.036(5) 0.059(6) 0.047(5) 0.030(5) 0.008(4) 0.001(4) C15B 0.035(5) 0.044(5) 0.093(9) 0.038(6) 0.006(5) -0.006(4) C16B 0.033(6) 0.017(4) 0.071(9) 0.010(6) -0.008(6) -0.002(3) C17B 0.016(6) 0.026(5) 0.037(10) 0.016(7) 0.004(7) 0.007(3) C18B 0.046(7) 0.018(5) 0.102(15) 0.024(9) -0.004(11) -0.010(4) C19B 0.056(15) 0.017(6) 0.08(2) -0.010(11) -0.030(17) -0.004(10) C20B 0.046(7) 0.033(5) 0.049(6) -0.017(4) -0.019(6) 0.012(5) C22B 0.075(8) 0.048(6) 0.049(6) -0.028(5) -0.020(5) 0.019(5) C23B 0.062(7) 0.075(7) 0.034(5) -0.023(5) 0.004(4) 0.023(5) C24B 0.043(6) 0.050(5) 0.027(4) -0.006(4) 0.001(4) 0.011(4) O1W 0.0204(13) 0.0370(14) 0.0282(13) -0.0056(11) 0.0045(10) -0.0012(10) O2W 0.066(2) 0.053(2) 0.075(3) 0.015(2) 0.027(2) 0.0099(19) _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 2.094(2) 1_655 ? Mn1 O10 2.193(3) 4_665 ? Mn1 O1W 2.211(2) . ? Mn1 O1 2.214(2) . ? Mn1 N2B 2.281(6) . ? Mn1 N1B 2.283(6) . ? Mn1 N1A 2.314(6) . ? Mn1 N2A 2.315(6) . ? Mn2 O2 2.080(2) . ? Mn2 O9 2.087(3) 4_665 ? Mn2 O6 2.105(2) 1_655 ? Mn2 N3B 2.225(10) . ? Mn2 N4B 2.248(14) . ? Mn2 N4A 2.256(13) . ? Mn2 N3A 2.283(10) . ? O1 C31 1.243(4) . ? O2 C31 1.253(4) . ? O3 C32 1.207(4) . ? O4 C32 1.303(4) . ? O5 C33 1.247(4) . ? O5 Mn1 2.094(2) 1_455 ? O6 C33 1.247(4) . ? O6 Mn2 2.105(2) 1_455 ? O9 C35 1.248(5) . ? O9 Mn2 2.086(3) 4_566 ? O10 C35 1.246(5) . ? O10 Mn1 2.193(3) 4_566 ? O11 C36 1.236(4) . ? O12 C36 1.263(4) . ? C25 C26 1.392(5) . ? C25 C30 1.400(5) . ? C25 C31 1.523(5) . ? C26 C27 1.399(5) . ? C26 C32 1.506(4) . ? C27 C28 1.395(5) . ? C27 C33 1.515(4) . ? C28 C29 1.392(5) . ? C28 C34 1.518(5) . ? C29 C30 1.406(5) . ? C29 C35 1.521(5) . ? C30 C36 1.498(4) . ? C34 O7B 1.237(6) . ? C34 O8B 1.253(6) . ? N1A C1A 1.334(10) . ? N1A C5A 1.352(10) . ? N2A C12A 1.316(10) . ? N2A C9A 1.371(13) . ? C1A C2A 1.409(11) . ? C2A C3A 1.336(14) . ? C3A C4A 1.413(13) . ? C4A C5A 1.415(11) . ? C4A C6A 1.428(12) . ? C5A C9A 1.438(13) . ? C6A C7A 1.442(12) . ? C7A C8A 1.362(10) . ? C8A C10A 1.397(13) . ? C8A C9A 1.403(14) . ? C10A C11A 1.346(13) . ? C11A C12A 1.428(11) . ? N3A C13A 1.317(14) . ? N3A C17A 1.34(3) . ? N4A C21A 1.342(16) . ? N4A C24A 1.342(15) . ? C13A C14A 1.412(11) . ? C14A C15A 1.368(13) . ? C15A C16A 1.410(16) . ? C16A C18A 1.41(2) . ? C16A C17A 1.46(2) . ? C17A C21A 1.44(2) . ? C18A C19A 1.34(3) . ? C19A C20A 1.42(2) . ? C20A C21A 1.398(12) . ? C20A C22A 1.404(14) . ? C22A C23A 1.355(13) . ? C23A C24A 1.395(10) . ? N1B C1B 1.318(10) . ? N1B C5B 1.361(13) . ? N2B C12B 1.327(10) . ? N2B C9B 1.361(10) . ? C1B C2B 1.402(11) . ? C2B C3B 1.360(14) . ? C2B C2B 2.029(17) 3_657 ? C3B C4B 1.403(13) . ? C4B C5B 1.393(15) . ? C5B C9B 1.444(13) . ? C7B C8B 1.445(12) . ? C8B C10B 1.399(13) . ? C8B C9B 1.403(11) . ? C10B C11B 1.376(14) . ? C11B C12B 1.384(11) . ? N3B C13B 1.344(13) . ? N3B C17B 1.38(3) . ? N4B C24B 1.292(16) . ? N4B C21B 1.387(17) . ? C13B C14B 1.392(11) . ? C14B C15B 1.354(15) . ? C15B C16B 1.443(18) . ? C16B C17B 1.37(3) . ? C16B C18B 1.46(2) . ? C17B C21B 1.416(16) . ? C18B C19B 1.36(2) . ? C19B C20B 1.42(2) . ? C20B C22B 1.375(17) . ? C20B C21B 1.412(13) . ? C22B C23B 1.371(16) . ? C23B C24B 1.402(12) . ? 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 Mn1 O10 86.62(10) 1_655 4_665 ? O5 Mn1 O1W 162.71(10) 1_655 . ? O10 Mn1 O1W 83.46(10) 4_665 . ? O5 Mn1 O1 94.86(10) 1_655 . ? O10 Mn1 O1 127.77(11) 4_665 . ? O1W Mn1 O1 80.27(9) . . ? O5 Mn1 N2B 84.74(17) 1_655 . ? O10 Mn1 N2B 76.06(18) 4_665 . ? O1W Mn1 N2B 106.43(17) . . ? O1 Mn1 N2B 156.15(17) . . ? O5 Mn1 N1B 114.66(18) 1_655 . ? O10 Mn1 N1B 139.75(18) 4_665 . ? O1W Mn1 N1B 81.74(18) . . ? O1 Mn1 N1B 86.03(17) . . ? N2B Mn1 N1B 72.7(2) . . ? O5 Mn1 N1A 91.64(17) 1_655 . ? O10 Mn1 N1A 155.31(17) 4_665 . ? O1W Mn1 N1A 103.24(17) . . ? O1 Mn1 N1A 76.92(17) . . ? N2B Mn1 N1A 79.3(2) . . ? N1B Mn1 N1A 25.3(2) . . ? O5 Mn1 N2A 108.03(18) 1_655 . ? O10 Mn1 N2A 85.83(17) 4_665 . ? O1W Mn1 N2A 85.38(18) . . ? O1 Mn1 N2A 140.90(18) . . ? N2B Mn1 N2A 24.7(2) . . ? N1B Mn1 N2A 55.9(2) . . ? N1A Mn1 N2A 71.3(2) . . ? O2 Mn2 O9 102.10(13) . 4_665 ? O2 Mn2 O6 101.24(10) . 1_655 ? O9 Mn2 O6 110.64(10) 4_665 1_655 ? O2 Mn2 N3B 148.5(3) . . ? O9 Mn2 N3B 83.2(3) 4_665 . ? O6 Mn2 N3B 105.9(2) 1_655 . ? O2 Mn2 N4B 93.0(3) . . ? O9 Mn2 N4B 155.9(4) 4_665 . ? O6 Mn2 N4B 84.2(3) 1_655 . ? N3B Mn2 N4B 74.3(5) . . ? O2 Mn2 N4A 84.3(3) . . ? O9 Mn2 N4A 151.6(3) 4_665 . ? O6 Mn2 N4A 94.8(3) 1_655 . ? N3B Mn2 N4A 77.7(4) . . ? N4B Mn2 N4A 12.5(3) . . ? O2 Mn2 N3A 154.3(3) . . ? O9 Mn2 N3A 93.5(3) 4_665 . ? O6 Mn2 N3A 92.0(2) 1_655 . ? N3B Mn2 N3A 15.01(19) . . ? N4B Mn2 N3A 66.3(4) . . ? N4A Mn2 N3A 72.6(4) . . ? C31 O1 Mn1 130.8(2) . . ? C31 O2 Mn2 136.7(2) . . ? C33 O5 Mn1 139.6(2) . 1_455 ? C33 O6 Mn2 134.1(2) . 1_455 ? C35 O9 Mn2 141.0(3) . 4_566 ? C35 O10 Mn1 132.3(3) . 4_566 ? C26 C25 C30 119.5(3) . . ? C26 C25 C31 117.8(3) . . ? C30 C25 C31 122.6(3) . . ? C25 C26 C27 121.0(3) . . ? C25 C26 C32 119.8(3) . . ? C27 C26 C32 119.2(3) . . ? C28 C27 C26 119.3(3) . . ? C28 C27 C33 120.4(3) . . ? C26 C27 C33 120.0(3) . . ? C29 C28 C27 120.2(3) . . ? C29 C28 C34 121.9(3) . . ? C27 C28 C34 117.8(3) . . ? C28 C29 C30 120.3(3) . . ? C28 C29 C35 117.2(3) . . ? C30 C29 C35 122.5(3) . . ? C25 C30 C29 119.6(3) . . ? C25 C30 C36 120.2(3) . . ? C29 C30 C36 120.2(3) . . ? O1 C31 O2 127.1(3) . . ? O1 C31 C25 118.9(3) . . ? O2 C31 C25 113.9(3) . . ? O3 C32 O4 125.2(3) . . ? O3 C32 C26 123.0(3) . . ? O4 C32 C26 111.7(3) . . ? O6 C33 O5 127.4(3) . . ? O6 C33 C27 118.6(3) . . ? O5 C33 C27 114.0(3) . . ? O7B C34 O8B 126.2(4) . . ? O7B C34 C28 115.8(4) . . ? O8B C34 C28 118.0(4) . . ? O10 C35 O9 126.7(4) . . ? O10 C35 C29 117.6(3) . . ? O9 C35 C29 115.5(3) . . ? O11 C36 O12 126.5(3) . . ? O11 C36 C30 118.2(3) . . ? O12 C36 C30 115.3(3) . . ? C1A N1A C5A 118.6(7) . . ? C1A N1A Mn1 124.7(5) . . ? C5A N1A Mn1 116.5(5) . . ? C12A N2A C9A 117.4(8) . . ? C12A N2A Mn1 125.9(5) . . ? C9A N2A Mn1 116.2(6) . . ? N1A C1A C2A 121.1(8) . . ? C3A C2A C1A 121.2(8) . . ? C2A C3A C4A 119.2(8) . . ? C3A C4A C5A 117.0(8) . . ? C3A C4A C6A 123.2(8) . . ? C5A C4A C6A 119.8(9) . . ? N1A C5A C4A 122.7(9) . . ? N1A C5A C9A 118.1(8) . . ? C4A C5A C9A 119.2(9) . . ? C4A C6A C7A 119.1(7) . . ? C8A C7A C6A 120.3(6) . . ? C7A C8A C10A 120.8(7) . . ? C7A C8A C9A 121.4(9) . . ? C10A C8A C9A 117.6(9) . . ? N2A C9A C8A 123.1(11) . . ? N2A C9A C5A 117.0(10) . . ? C8A C9A C5A 119.8(10) . . ? C11A C10A C8A 119.8(7) . . ? C10A C11A C12A 119.6(8) . . ? N2A C12A C11A 122.5(8) . . ? C13A N3A C17A 121.2(12) . . ? C13A N3A Mn2 125.0(7) . . ? C17A N3A Mn2 113.9(11) . . ? C21A N4A C24A 115.7(11) . . ? C21A N4A Mn2 117.9(9) . . ? C24A N4A Mn2 126.3(8) . . ? N3A C13A C14A 121.8(9) . . ? C15A C14A C13A 120.0(8) . . ? C14A C15A C16A 118.8(8) . . ? C15A C16A C18A 125.2(12) . . ? C15A C16A C17A 118.0(12) . . ? C18A C16A C17A 116.8(14) . . ? N3A C17A C21A 120.9(15) . . ? N3A C17A C16A 120.2(16) . . ? C21A C17A C16A 118.9(15) . . ? C19A C18A C16A 124.2(18) . . ? C18A C19A C20A 119.7(17) . . ? C21A C20A C22A 116.5(9) . . ? C21A C20A C19A 120.4(11) . . ? C22A C20A C19A 123.1(11) . . ? N4A C21A C20A 125.4(10) . . ? N4A C21A C17A 114.7(12) . . ? C20A C21A C17A 119.8(11) . . ? C23A C22A C20A 119.0(7) . . ? C22A C23A C24A 120.1(8) . . ? N4A C24A C23A 123.0(9) . . ? C1B N1B C5B 118.0(8) . . ? C1B N1B Mn1 126.2(5) . . ? C5B N1B Mn1 115.6(7) . . ? C12B N2B C9B 117.7(7) . . ? C12B N2B Mn1 126.1(5) . . ? C9B N2B Mn1 116.2(5) . . ? N1B C1B C2B 122.7(8) . . ? C3B C2B C1B 119.5(8) . . ? C3B C2B C2B 101.5(9) . 3_657 ? C1B C2B C2B 77.9(6) . 3_657 ? C2B C3B C4B 119.2(7) . . ? C5B C4B C3B 117.7(9) . . ? N1B C5B C4B 122.8(12) . . ? N1B C5B C9B 118.1(10) . . ? C4B C5B C9B 119.1(10) . . ? C10B C8B C9B 117.3(8) . . ? C10B C8B C7B 123.6(8) . . ? C9B C8B C7B 119.1(9) . . ? N2B C9B C8B 123.0(9) . . ? N2B C9B C5B 117.1(8) . . ? C8B C9B C5B 119.9(9) . . ? C11B C10B C8B 119.4(7) . . ? C10B C11B C12B 119.5(8) . . ? N2B C12B C11B 123.1(8) . . ? C13B N3B C17B 116.7(11) . . ? C13B N3B Mn2 126.4(7) . . ? C17B N3B Mn2 116.8(10) . . ? C24B N4B C21B 119.6(12) . . ? C24B N4B Mn2 126.9(10) . . ? C21B N4B Mn2 113.4(9) . . ? N3B C13B C14B 122.2(9) . . ? C15B C14B C13B 120.6(9) . . ? C14B C15B C16B 119.7(8) . . ? C17B C16B C15B 115.7(12) . . ? C17B C16B C18B 121.3(15) . . ? C15B C16B C18B 123.0(10) . . ? C16B C17B N3B 125.1(15) . . ? C16B C17B C21B 119.7(18) . . ? N3B C17B C21B 115.1(16) . . ? C19B C18B C16B 117.8(17) . . ? C18B C19B C20B 122.0(19) . . ? C22B C20B C21B 118.9(11) . . ? C22B C20B C19B 121.8(12) . . ? C21B C20B C19B 119.2(13) . . ? N4B C21B C20B 119.9(11) . . ? N4B C21B C17B 120.1(13) . . ? C20B C21B C17B 119.9(13) . . ? C23B C22B C20B 119.6(9) . . ? C22B C23B C24B 119.0(9) . . ? N4B C24B C23B 122.8(11) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 71.34 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.619 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.070