Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jose Galan-Mascaros' _publ_contact_author_address ; Instituto de Ciencia Molecular Universitat de Valencia Poligono de la Coma, s/n Paterna Valencia 46980 SPAIN ; _publ_contact_author_email JOSE.R.GALAN@UV.ES _publ_section_title ; Heptacoordinated MnII in oxalate-based bimetallic 2D magnets: Synthesis and characterisation of [Mn(L)6][Mn(CH3OH)MIII(ox)3]2 (MIII = Cr, Rh; ox = oxalate dianion; L = H2O, CH3OH) ; loop_ _publ_author_name 'Jose Galan-Mascaros' 'Eugenio Coronado' 'Carlos Marti-Gastaldo' 'Ana Murcia Martinez' data_2 _database_code_depnum_ccdc_archive 'CCDC 600903' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H40 Cr2 Mn3 O34' _chemical_formula_weight 1117.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 9.0730(1) _cell_length_b 14.2670(2) _cell_length_c 16.8850(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.4710(6) _cell_angle_gamma 90.00 _cell_volume 2155.88(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17611 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'square prism' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1134 _exptl_absorpt_coefficient_mu 1.447 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.964 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17611 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4822 _reflns_number_gt 3580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SIR97 (Giacovazzo et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalMaker 7.0.3' _computing_publication_material SHELXL-97 _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^)+(0.0860P)^2^+1.9335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0043(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4822 _refine_ls_number_parameters 266 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1477 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Cr1 Cr 0.05284(6) 0.22608(4) -0.26596(3) 0.02678(18) Uani 1 1 d . . . Mn1 Mn 0.59986(6) 0.16510(4) -0.08687(3) 0.03020(18) Uani 1 1 d . . . Mn2 Mn -0.5000 0.0000 -0.5000 0.0348(2) Uani 1 2 d S . . O1 O 0.1645(3) 0.12181(18) -0.20615(14) 0.0312(6) Uani 1 1 d . . . O2 O 0.3922(3) 0.09337(18) -0.13575(15) 0.0323(6) Uani 1 1 d . . . O3 O 0.2447(3) 0.29354(18) -0.23737(16) 0.0339(6) Uani 1 1 d . . . O4 O 0.4649(3) 0.27541(18) -0.15754(17) 0.0370(6) Uani 1 1 d . . . O5 O -0.1402(3) 0.15775(18) -0.27695(14) 0.0300(5) Uani 1 1 d . . . O6 O -0.3252(3) 0.1303(2) -0.20692(16) 0.0361(6) Uani 1 1 d . . . O7 O -0.0088(3) 0.27145(17) -0.16476(15) 0.0310(6) Uani 1 1 d . . . O8 O -0.1803(3) 0.2400(2) -0.08746(15) 0.0349(6) Uani 1 1 d . . . O9 O 0.1072(3) 0.18258(18) -0.36703(15) 0.0335(6) Uani 1 1 d . . . O10 O -0.0386(3) 0.33114(18) -0.33389(16) 0.0349(6) Uani 1 1 d . . . O11 O 0.1224(4) 0.2350(2) -0.48930(17) 0.0467(7) Uani 1 1 d . . . O12 O -0.0527(4) 0.3830(2) -0.46047(19) 0.0533(8) Uani 1 1 d . . . O13 O 0.7132(3) 0.0422(2) -0.03627(18) 0.0448(7) Uani 1 1 d . . . O21 O -0.2870(3) -0.0083(2) -0.4215(2) 0.0533(8) Uani 1 1 d . . . O22 O -0.5947(4) -0.0537(2) -0.39829(18) 0.0455(7) Uani 1 1 d . . . O23 O -0.5387(4) 0.1438(2) -0.46845(18) 0.0498(8) Uani 1 1 d D . . C1 C 0.2973(4) 0.1441(2) -0.1755(2) 0.0273(7) Uani 1 1 d . . . C2 C 0.3423(4) 0.2460(3) -0.1909(2) 0.0302(7) Uani 1 1 d . . . C3 C -0.2067(4) 0.1673(2) -0.2165(2) 0.0278(7) Uani 1 1 d . . . C4 C -0.1263(4) 0.2314(3) -0.1498(2) 0.0282(7) Uani 1 1 d . . . C5 C 0.0800(4) 0.2420(3) -0.4235(2) 0.0319(8) Uani 1 1 d . . . C6 C -0.0124(5) 0.3276(3) -0.4053(2) 0.0359(8) Uani 1 1 d . . . C13 C 0.8164(6) 0.0428(4) 0.0385(3) 0.0598(13) Uani 1 1 d . . . H131 H 0.8860 0.0934 0.0383 0.090 Uiso 1 1 calc . . . H132 H 0.8696 -0.0156 0.0447 0.090 Uiso 1 1 calc . . . H133 H 0.7621 0.0509 0.0823 0.090 Uiso 1 1 calc . . . C21 C -0.1431(6) 0.0005(4) -0.4423(4) 0.0691(15) Uani 1 1 d . . . H211 H -0.1150 -0.0577 -0.4641 0.104 Uiso 1 1 calc . . . H212 H -0.0724 0.0161 -0.3954 0.104 Uiso 1 1 calc . . . H213 H -0.1440 0.0492 -0.4817 0.104 Uiso 1 1 calc . . . C22 C -0.6429(8) -0.0015(4) -0.3344(3) 0.0677(16) Uani 1 1 d . . . H221 H -0.5615 0.0043 -0.2905 0.102 Uiso 1 1 calc . . . H222 H -0.7244 -0.0336 -0.3166 0.102 Uiso 1 1 calc . . . H223 H -0.6750 0.0598 -0.3535 0.102 Uiso 1 1 calc . . . C23 C -0.4752(13) 0.2020(7) -0.4040(6) 0.0578(19) Uiso 0.50 1 d PD A 1 H231 H -0.4085 0.1658 -0.3658 0.087 Uiso 0.50 1 calc P B 1 H232 H -0.5532 0.2277 -0.3784 0.087 Uiso 0.50 1 calc P C 1 H233 H -0.4209 0.2521 -0.4240 0.087 Uiso 0.50 1 calc P D 1 C24 C -0.4268(11) 0.2069(7) -0.4286(7) 0.0578(19) Uiso 0.50 1 d PD A 2 H241 H -0.4733 0.2532 -0.3996 0.087 Uiso 0.50 1 calc P E 2 H242 H -0.3776 0.2372 -0.4677 0.087 Uiso 0.50 1 calc P F 2 H243 H -0.3549 0.1723 -0.3918 0.087 Uiso 0.50 1 calc P G 2 O101 O 0.1224(6) 0.0762(4) -0.7844(3) 0.0841(15) Uiso 0.50 1 d P H 3 C102 C 0.2483(8) 0.0863(5) -0.7311(4) 0.1036(19) Uiso 0.50 1 d P H 3 H1 H 0.2254 0.1150 -0.6832 0.155 Uiso 0.50 1 calc P I 3 H2 H 0.3171 0.1252 -0.7537 0.155 Uiso 0.50 1 calc P J 3 H3 H 0.2925 0.0259 -0.7183 0.155 Uiso 0.50 1 calc P K 3 O102 O 0.2483(8) 0.0863(5) -0.7311(4) 0.1036(19) Uiso 0.50 1 d P L 4 C101 C 0.1224(6) 0.0762(4) -0.7844(3) 0.0841(15) Uiso 0.50 1 d P L 4 H4 H 0.0485 0.0450 -0.7593 0.126 Uiso 0.50 1 calc P M 4 H5 H 0.1428 0.0396 -0.8291 0.126 Uiso 0.50 1 calc P N 4 H6 H 0.0859 0.1368 -0.8030 0.126 Uiso 0.50 1 calc P O 4 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 Cr1 0.0260(3) 0.0311(3) 0.0242(3) 0.0015(2) 0.0069(2) 0.0006(2) Mn1 0.0270(3) 0.0334(3) 0.0305(3) -0.0034(2) 0.0056(2) -0.0048(2) Mn2 0.0370(5) 0.0340(4) 0.0327(4) 0.0035(3) 0.0037(3) 0.0058(3) O1 0.0315(13) 0.0329(13) 0.0289(13) 0.0034(10) 0.0038(10) -0.0057(10) O2 0.0302(13) 0.0316(13) 0.0338(13) 0.0044(11) 0.0013(10) -0.0024(10) O3 0.0312(13) 0.0326(13) 0.0393(14) 0.0060(11) 0.0095(11) -0.0021(11) O4 0.0286(13) 0.0351(14) 0.0458(16) 0.0024(12) 0.0015(11) -0.0051(11) O5 0.0271(12) 0.0378(14) 0.0253(12) -0.0050(10) 0.0047(9) -0.0007(10) O6 0.0294(14) 0.0456(15) 0.0339(14) -0.0086(12) 0.0070(11) -0.0093(11) O7 0.0303(13) 0.0339(14) 0.0297(13) -0.0053(10) 0.0078(10) -0.0063(10) O8 0.0319(14) 0.0448(15) 0.0293(13) -0.0078(11) 0.0091(10) -0.0089(11) O9 0.0382(14) 0.0337(14) 0.0305(13) 0.0046(11) 0.0111(11) 0.0034(11) O10 0.0349(14) 0.0354(14) 0.0349(14) 0.0032(11) 0.0070(11) 0.0080(11) O11 0.063(2) 0.0468(17) 0.0335(15) 0.0041(13) 0.0192(13) 0.0017(14) O12 0.074(2) 0.0399(16) 0.0400(16) 0.0091(13) -0.0095(15) 0.0043(15) O13 0.0476(17) 0.0422(16) 0.0429(16) 0.0053(13) 0.0026(13) -0.0011(13) O21 0.0407(17) 0.061(2) 0.0535(19) -0.0052(15) -0.0047(14) 0.0085(15) O22 0.0593(19) 0.0375(15) 0.0428(16) 0.0046(12) 0.0172(13) 0.0127(13) O23 0.065(2) 0.0383(15) 0.0406(16) -0.0028(13) -0.0075(14) 0.0138(14) C1 0.0278(17) 0.0308(17) 0.0246(16) -0.0006(14) 0.0082(13) -0.0015(14) C2 0.0308(18) 0.0312(18) 0.0302(18) 0.0023(14) 0.0095(14) -0.0035(15) C3 0.0228(16) 0.0328(18) 0.0275(17) -0.0009(14) 0.0035(13) 0.0001(13) C4 0.0245(17) 0.0356(19) 0.0251(16) -0.0001(14) 0.0058(13) 0.0000(14) C5 0.0333(19) 0.0353(19) 0.0280(18) 0.0039(15) 0.0080(14) -0.0013(15) C6 0.041(2) 0.0301(19) 0.036(2) 0.0027(16) 0.0041(16) -0.0044(16) C13 0.052(3) 0.058(3) 0.065(3) 0.018(3) -0.003(2) -0.007(2) C21 0.043(3) 0.074(4) 0.087(4) -0.024(3) 0.000(3) -0.002(3) C22 0.104(4) 0.047(3) 0.063(3) 0.008(2) 0.043(3) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O9 1.954(3) . ? Cr1 O3 1.978(3) . ? Cr1 O1 1.981(3) . ? Cr1 O10 1.984(3) . ? Cr1 O5 1.986(3) . ? Cr1 O7 1.991(2) . ? Mn1 O13 2.138(3) . ? Mn1 O11 2.162(3) 4_666 ? Mn1 O2 2.183(3) . ? Mn1 O4 2.218(3) . ? Mn1 O8 2.264(3) 1_655 ? Mn1 O6 2.296(3) 1_655 ? Mn2 O21 2.159(3) 3_454 ? Mn2 O21 2.159(3) . ? Mn2 O23 2.163(3) 3_454 ? Mn2 O23 2.163(3) . ? Mn2 O22 2.182(3) 3_454 ? Mn2 O22 2.182(3) . ? O1 C1 1.270(4) . ? O2 C1 1.235(4) . ? O3 C2 1.278(5) . ? O4 C2 1.234(4) . ? O5 C3 1.276(4) . ? O6 C3 1.232(4) . ? O6 Mn1 2.296(3) 1_455 ? O7 C4 1.272(4) . ? O8 C4 1.237(4) . ? O8 Mn1 2.264(3) 1_455 ? O9 C5 1.269(4) . ? O10 C6 1.267(5) . ? O11 C5 1.238(5) . ? O11 Mn1 2.162(3) 4_565 ? O12 C6 1.231(5) . ? O13 C13 1.443(6) . ? O21 C21 1.413(7) . ? O22 C22 1.437(6) . ? O23 C23 1.414(9) . ? O23 C24 1.438(9) . ? C1 C2 1.544(5) . ? C3 C4 1.538(5) . ? C5 C6 1.540(6) . ? C13 H131 0.9600 . ? C13 H132 0.9600 . ? C13 H133 0.9600 . ? C21 H211 0.9600 . ? C21 H212 0.9600 . ? C21 H213 0.9600 . ? C22 H221 0.9600 . ? C22 H222 0.9600 . ? C22 H223 0.9600 . ? C23 H231 0.9600 . ? C23 H232 0.9600 . ? C23 H233 0.9600 . ? C24 H241 0.9600 . ? C24 H242 0.9600 . ? C24 H243 0.9600 . ? O101 C102 1.340(8) . ? C102 H1 0.9600 . ? C102 H2 0.9600 . ? C102 H3 0.9600 . ? 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 O9 Cr1 O3 91.68(11) . . ? O9 Cr1 O1 91.45(11) . . ? O3 Cr1 O1 83.40(10) . . ? O9 Cr1 O10 82.91(11) . . ? O3 Cr1 O10 92.33(11) . . ? O1 Cr1 O10 172.85(11) . . ? O9 Cr1 O5 96.20(11) . . ? O3 Cr1 O5 171.34(11) . . ? O1 Cr1 O5 92.77(10) . . ? O10 Cr1 O5 92.21(11) . . ? O9 Cr1 O7 178.24(11) . . ? O3 Cr1 O7 89.57(10) . . ? O1 Cr1 O7 89.94(11) . . ? O10 Cr1 O7 95.79(11) . . ? O5 Cr1 O7 82.64(10) . . ? O13 Mn1 O11 104.89(12) . 4_666 ? O13 Mn1 O2 95.45(10) . . ? O11 Mn1 O2 124.36(11) 4_666 . ? O13 Mn1 O4 169.54(11) . . ? O11 Mn1 O4 85.23(11) 4_666 . ? O2 Mn1 O4 76.32(9) . . ? O13 Mn1 O8 91.30(11) . 1_655 ? O11 Mn1 O8 73.71(11) 4_666 1_655 ? O2 Mn1 O8 157.75(10) . 1_655 ? O4 Mn1 O8 94.10(10) . 1_655 ? O13 Mn1 O6 89.01(11) . 1_655 ? O11 Mn1 O6 144.15(11) 4_666 1_655 ? O2 Mn1 O6 85.84(9) . 1_655 ? O4 Mn1 O6 84.02(10) . 1_655 ? O8 Mn1 O6 73.08(9) 1_655 1_655 ? O21 Mn2 O21 180.0 3_454 . ? O21 Mn2 O23 93.79(12) 3_454 3_454 ? O21 Mn2 O23 86.22(12) . 3_454 ? O21 Mn2 O23 86.22(12) 3_454 . ? O21 Mn2 O23 93.78(12) . . ? O23 Mn2 O23 179.997(1) 3_454 . ? O21 Mn2 O22 85.75(13) 3_454 3_454 ? O21 Mn2 O22 94.25(13) . 3_454 ? O23 Mn2 O22 92.20(12) 3_454 3_454 ? O23 Mn2 O22 87.80(12) . 3_454 ? O21 Mn2 O22 94.25(13) 3_454 . ? O21 Mn2 O22 85.75(13) . . ? O23 Mn2 O22 87.80(12) 3_454 . ? O23 Mn2 O22 92.20(12) . . ? O22 Mn2 O22 180.0 3_454 . ? C1 O1 Cr1 113.0(2) . . ? C1 O2 Mn1 114.3(2) . . ? C2 O3 Cr1 112.7(2) . . ? C2 O4 Mn1 112.4(2) . . ? C3 O5 Cr1 113.5(2) . . ? C3 O6 Mn1 114.5(2) . 1_455 ? C4 O7 Cr1 112.8(2) . . ? C4 O8 Mn1 115.4(2) . 1_455 ? C5 O9 Cr1 113.5(2) . . ? C6 O10 Cr1 113.2(2) . . ? C5 O11 Mn1 128.8(3) . 4_565 ? C13 O13 Mn1 123.0(3) . . ? C21 O21 Mn2 127.8(3) . . ? C22 O22 Mn2 128.0(3) . . ? C23 O23 C24 26.6(5) . . ? C23 O23 Mn2 133.2(5) . . ? C24 O23 Mn2 125.3(5) . . ? O2 C1 O1 127.2(3) . . ? O2 C1 C2 117.6(3) . . ? O1 C1 C2 115.3(3) . . ? O4 C2 O3 125.6(3) . . ? O4 C2 C1 119.1(3) . . ? O3 C2 C1 115.3(3) . . ? O6 C3 O5 126.7(3) . . ? O6 C3 C4 118.5(3) . . ? O5 C3 C4 114.8(3) . . ? O8 C4 O7 125.9(3) . . ? O8 C4 C3 118.4(3) . . ? O7 C4 C3 115.7(3) . . ? O11 C5 O9 124.7(4) . . ? O11 C5 C6 120.2(3) . . ? O9 C5 C6 115.1(3) . . ? O12 C6 O10 128.0(4) . . ? O12 C6 C5 117.5(4) . . ? O10 C6 C5 114.5(3) . . ? O13 C13 H131 109.5 . . ? O13 C13 H132 109.5 . . ? H131 C13 H132 109.5 . . ? O13 C13 H133 109.5 . . ? H131 C13 H133 109.5 . . ? H132 C13 H133 109.5 . . ? O21 C21 H211 109.5 . . ? O21 C21 H212 109.5 . . ? H211 C21 H212 109.5 . . ? O21 C21 H213 109.5 . . ? H211 C21 H213 109.5 . . ? H212 C21 H213 109.5 . . ? O22 C22 H221 109.5 . . ? O22 C22 H222 109.5 . . ? H221 C22 H222 109.5 . . ? O22 C22 H223 109.5 . . ? H221 C22 H223 109.5 . . ? H222 C22 H223 109.5 . . ? O23 C23 H231 109.5 . . ? O23 C23 H232 109.5 . . ? H231 C23 H232 109.5 . . ? O23 C23 H233 109.5 . . ? H231 C23 H233 109.5 . . ? H232 C23 H233 109.5 . . ? O23 C24 H241 109.5 . . ? O23 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? O23 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? O101 C102 H1 109.5 . . ? O101 C102 H2 109.5 . . ? H1 C102 H2 109.5 . . ? O101 C102 H3 109.5 . . ? H1 C102 H3 109.5 . . ? H2 C102 H3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.407 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.099 ###END data_3 _database_code_depnum_ccdc_archive 'CCDC 600904' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H39 Mn3 O35.50 Rh2' _chemical_formula_weight 1218.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 9.5140(1) _cell_length_b 16.0720(3) _cell_length_c 14.9480(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.3560(7) _cell_angle_gamma 90.00 _cell_volume 2204.08(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4953 _cell_measurement_theta_min 4.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'square prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.977 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4953 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4953 _reflns_number_gt 3893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SIR97 (Giacovazzo et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalMaker 7.0.3' _computing_publication_material SHELXL-97 _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^)+(0.0889P)^2^+5.5400P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4953 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1300 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.002 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 Rh1 Rh -0.01177(4) 0.21904(2) 0.23568(2) 0.01865(13) Uani 1 1 d . . . Mn1 Mn 0.45356(7) 0.05424(4) 0.16591(5) 0.02062(18) Uani 1 1 d . . . Mn3 Mn 0.5000 0.5000 0.0000 0.0291(3) Uani 1 2 d S . . O1 O 0.1370(3) 0.2378(2) 0.1647(2) 0.0219(7) Uani 1 1 d . . . O2 O 0.1058(4) 0.1154(2) 0.2805(2) 0.0252(7) Uani 1 1 d . . . O3 O -0.1439(3) 0.1488(2) 0.1358(2) 0.0243(7) Uani 1 1 d . . . O4 O -0.1664(3) 0.1969(2) 0.3043(2) 0.0218(7) Uani 1 1 d . . . O5 O -0.1150(3) 0.3271(2) 0.1919(2) 0.0253(7) Uani 1 1 d . . . O6 O 0.1121(3) 0.29062(19) 0.3360(2) 0.0227(7) Uani 1 1 d . . . O7 O -0.3521(3) 0.0776(2) 0.1134(2) 0.0247(7) Uani 1 1 d . . . O8 O -0.3854(3) 0.1372(2) 0.2751(2) 0.0248(7) Uani 1 1 d . . . O9 O 0.3342(3) 0.1747(2) 0.1422(2) 0.0234(7) Uani 1 1 d . . . O10 O 0.2974(4) 0.0496(2) 0.2546(3) 0.0308(8) Uani 1 1 d . . . O11 O -0.0928(3) 0.4612(2) 0.2311(2) 0.0277(7) Uani 1 1 d . . . O12 O 0.1358(4) 0.4247(2) 0.3744(2) 0.0281(7) Uani 1 1 d . . . O13 O 0.3487(4) 0.0517(2) 0.0128(2) 0.0289(7) Uani 1 1 d . . . O21 O 0.3792(4) 0.5076(3) -0.1438(3) 0.0392(9) Uani 1 1 d . . . O22 O 0.4837(5) 0.3658(3) -0.0180(3) 0.0439(10) Uani 1 1 d . . . O23 O 0.3023(6) 0.5024(4) 0.0446(4) 0.0677(15) Uani 1 1 d . . . C1 C 0.2308(5) 0.1796(3) 0.1775(3) 0.0188(9) Uani 1 1 d . . . C2 C 0.2114(5) 0.1078(3) 0.2422(3) 0.0222(9) Uani 1 1 d . . . C3 C -0.2559(5) 0.1245(3) 0.1596(3) 0.0207(9) Uani 1 1 d . . . C4 C -0.2732(5) 0.1550(3) 0.2541(3) 0.0198(9) Uani 1 1 d . . . C5 C -0.0543(5) 0.3875(3) 0.2422(3) 0.0223(9) Uani 1 1 d . . . C6 C 0.0770(5) 0.3672(3) 0.3248(3) 0.0222(9) Uani 1 1 d . . . C13 C 0.3134(7) 0.1163(4) -0.0525(4) 0.0429(14) Uani 1 1 d . . . H131 H 0.2681 0.0935 -0.1126 0.064 Uiso 1 1 calc . . . H132 H 0.4006 0.1454 -0.0546 0.064 Uiso 1 1 calc . . . H133 H 0.2473 0.1542 -0.0350 0.064 Uiso 1 1 calc . . . C22 C 0.5590(8) 0.2987(4) 0.0358(4) 0.0470(15) Uani 1 1 d . . . H221 H 0.5240 0.2470 0.0060 0.070 Uiso 1 1 calc . . . H222 H 0.5423 0.3000 0.0964 0.070 Uiso 1 1 calc . . . H223 H 0.6615 0.3037 0.0415 0.070 Uiso 1 1 calc . . . C23 C 0.1912(15) 0.4457(13) 0.0357(14) 0.162(7) Uani 1 1 d . . . H231 H 0.1164 0.4690 0.0603 0.242 Uiso 1 1 calc . . . H232 H 0.2285 0.3960 0.0693 0.242 Uiso 1 1 calc . . . H233 H 0.1513 0.4325 -0.0287 0.242 Uiso 1 1 calc . . . O101 O 0.5060(7) 0.4358(4) 0.2726(4) 0.0766(16) Uiso 1 1 d . A 1 C101 C 0.4380(13) 0.3578(8) 0.2630(8) 0.102(3) Uiso 1 1 d . A 1 O102 O 0.0383(12) 0.0226(7) 0.0768(8) 0.068(3) Uiso 0.50 1 d P B 2 O103 O 0.0000 0.0000 0.0000 0.080(5) Uiso 0.50 2 d SP . . 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 Rh1 0.01531(19) 0.0177(2) 0.0235(2) -0.00295(13) 0.00623(13) -0.00159(12) Mn1 0.0166(3) 0.0184(4) 0.0266(4) -0.0012(3) 0.0052(3) 0.0007(3) Mn3 0.0292(6) 0.0297(6) 0.0255(5) 0.0018(4) 0.0018(4) 0.0050(4) O1 0.0200(15) 0.0213(16) 0.0261(17) 0.0031(13) 0.0088(13) 0.0009(13) O2 0.0270(17) 0.0198(16) 0.0343(18) 0.0012(13) 0.0180(14) -0.0006(13) O3 0.0222(16) 0.0270(17) 0.0255(17) -0.0062(13) 0.0094(13) -0.0023(13) O4 0.0183(15) 0.0222(16) 0.0252(16) -0.0074(13) 0.0064(13) -0.0036(13) O5 0.0183(15) 0.0244(17) 0.0297(18) -0.0032(14) 0.0005(13) -0.0001(13) O6 0.0194(16) 0.0200(16) 0.0263(17) -0.0014(12) 0.0017(13) -0.0019(12) O7 0.0221(16) 0.0234(17) 0.0284(17) -0.0077(13) 0.0065(13) -0.0046(13) O8 0.0183(15) 0.0276(17) 0.0303(18) -0.0058(14) 0.0096(13) -0.0019(13) O9 0.0203(15) 0.0216(17) 0.0313(17) -0.0005(13) 0.0123(13) 0.0009(13) O10 0.0347(19) 0.0231(18) 0.040(2) 0.0075(14) 0.0198(16) 0.0085(15) O11 0.0215(16) 0.0203(17) 0.038(2) 0.0014(14) 0.0022(14) 0.0023(13) O12 0.0266(17) 0.0220(17) 0.0308(18) -0.0030(14) -0.0013(14) -0.0031(14) O13 0.0328(18) 0.0233(17) 0.0278(18) -0.0006(13) 0.0030(14) 0.0022(14) O21 0.036(2) 0.042(2) 0.035(2) 0.0010(17) 0.0017(16) 0.0051(17) O22 0.048(2) 0.035(2) 0.037(2) -0.0017(17) -0.0084(18) 0.0051(18) O23 0.047(3) 0.081(4) 0.083(4) 0.011(3) 0.030(3) 0.008(3) C1 0.018(2) 0.018(2) 0.019(2) -0.0033(16) 0.0020(17) -0.0026(17) C2 0.026(2) 0.017(2) 0.024(2) -0.0036(17) 0.0073(18) -0.0042(18) C3 0.020(2) 0.018(2) 0.024(2) -0.0028(17) 0.0057(17) 0.0015(17) C4 0.018(2) 0.016(2) 0.025(2) -0.0003(17) 0.0057(17) 0.0030(16) C5 0.017(2) 0.024(2) 0.028(2) -0.0029(19) 0.0088(18) -0.0013(18) C6 0.019(2) 0.023(2) 0.026(2) -0.0014(18) 0.0093(18) -0.0038(18) C13 0.061(4) 0.033(3) 0.034(3) 0.002(2) 0.012(3) 0.006(3) C22 0.055(4) 0.039(3) 0.038(3) -0.001(3) -0.003(3) 0.001(3) C23 0.080(8) 0.218(18) 0.194(17) -0.083(14) 0.050(10) -0.043(10) _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 Rh1 O1 2.004(3) . ? Rh1 O6 2.006(3) . ? Rh1 O5 2.017(3) . ? Rh1 O2 2.020(3) . ? Rh1 O3 2.022(3) . ? Rh1 O4 2.035(3) . ? Mn1 O7 2.223(3) 1_655 ? Mn1 O9 2.226(3) . ? Mn1 O10 2.239(3) . ? Mn1 O13 2.242(4) . ? Mn1 O12 2.269(3) 2_545 ? Mn1 O11 2.297(3) 2_545 ? Mn1 O8 2.337(3) 1_655 ? Mn3 O21 2.155(4) . ? Mn3 O21 2.155(4) 3_665 ? Mn3 O23 2.156(5) 3_665 ? Mn3 O23 2.156(5) . ? Mn3 O22 2.174(4) . ? Mn3 O22 2.174(4) 3_665 ? O1 C1 1.272(6) . ? O2 C2 1.287(6) . ? O3 C3 1.271(5) . ? O4 C4 1.283(5) . ? O5 C5 1.270(6) . ? O6 C6 1.275(6) . ? O7 C3 1.244(5) . ? O7 Mn1 2.224(3) 1_455 ? O8 C4 1.224(5) . ? O8 Mn1 2.337(3) 1_455 ? O9 C1 1.235(5) . ? O10 C2 1.225(6) . ? O11 C5 1.238(6) . ? O11 Mn1 2.297(3) 2 ? O12 C6 1.224(6) . ? O12 Mn1 2.269(3) 2 ? O13 C13 1.404(7) . ? O22 C22 1.421(7) . ? O23 C23 1.375(16) . ? C1 C2 1.547(6) . ? C3 C4 1.544(6) . ? C5 C6 1.540(7) . ? C13 H131 0.9600 . ? C13 H132 0.9600 . ? C13 H133 0.9600 . ? C22 H221 0.9600 . ? C22 H222 0.9600 . ? C22 H223 0.9600 . ? C23 H231 0.9600 . ? C23 H232 0.9601 . ? C23 H233 0.9600 . ? O101 C101 1.400(14) . ? O102 O103 1.167(12) . ? O103 O102 1.167(12) 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 O1 Rh1 O6 87.25(13) . . ? O1 Rh1 O5 92.86(13) . . ? O6 Rh1 O5 83.56(13) . . ? O1 Rh1 O2 83.85(13) . . ? O6 Rh1 O2 93.50(13) . . ? O5 Rh1 O2 175.71(13) . . ? O1 Rh1 O3 94.66(13) . . ? O6 Rh1 O3 177.67(13) . . ? O5 Rh1 O3 94.99(13) . . ? O2 Rh1 O3 88.04(13) . . ? O1 Rh1 O4 177.95(12) . . ? O6 Rh1 O4 94.79(13) . . ? O5 Rh1 O4 87.67(13) . . ? O2 Rh1 O4 95.71(13) . . ? O3 Rh1 O4 83.32(12) . . ? O7 Mn1 O9 103.52(12) 1_655 . ? O7 Mn1 O10 163.49(14) 1_655 . ? O9 Mn1 O10 74.49(12) . . ? O7 Mn1 O13 80.19(13) 1_655 . ? O9 Mn1 O13 77.49(12) . . ? O10 Mn1 O13 114.72(14) . . ? O7 Mn1 O12 110.47(13) 1_655 2_545 ? O9 Mn1 O12 128.06(12) . 2_545 ? O10 Mn1 O12 82.27(13) . 2_545 ? O13 Mn1 O12 71.21(12) . 2_545 ? O7 Mn1 O11 87.75(12) 1_655 2_545 ? O9 Mn1 O11 148.44(12) . 2_545 ? O10 Mn1 O11 86.37(13) . 2_545 ? O13 Mn1 O11 133.93(13) . 2_545 ? O12 Mn1 O11 71.95(12) 2_545 2_545 ? O7 Mn1 O8 72.38(11) 1_655 1_655 ? O9 Mn1 O8 80.05(12) . 1_655 ? O10 Mn1 O8 91.20(13) . 1_655 ? O13 Mn1 O8 139.07(13) . 1_655 ? O12 Mn1 O8 147.03(12) 2_545 1_655 ? O11 Mn1 O8 75.42(12) 2_545 1_655 ? O21 Mn3 O21 180.0 . 3_665 ? O21 Mn3 O23 88.35(19) . 3_665 ? O21 Mn3 O23 91.65(19) 3_665 3_665 ? O21 Mn3 O23 91.65(19) . . ? O21 Mn3 O23 88.35(19) 3_665 . ? O23 Mn3 O23 180.0 3_665 . ? O21 Mn3 O22 86.05(14) . . ? O21 Mn3 O22 93.95(14) 3_665 . ? O23 Mn3 O22 89.1(2) 3_665 . ? O23 Mn3 O22 90.9(2) . . ? O21 Mn3 O22 93.95(14) . 3_665 ? O21 Mn3 O22 86.05(14) 3_665 3_665 ? O23 Mn3 O22 90.9(2) 3_665 3_665 ? O23 Mn3 O22 89.1(2) . 3_665 ? O22 Mn3 O22 180.0 . 3_665 ? C1 O1 Rh1 112.1(3) . . ? C2 O2 Rh1 111.0(3) . . ? C3 O3 Rh1 111.6(3) . . ? C4 O4 Rh1 111.3(3) . . ? C5 O5 Rh1 111.1(3) . . ? C6 O6 Rh1 112.0(3) . . ? C3 O7 Mn1 117.7(3) . 1_455 ? C4 O8 Mn1 114.2(3) . 1_455 ? C1 O9 Mn1 114.7(3) . . ? C2 O10 Mn1 114.0(3) . . ? C5 O11 Mn1 115.8(3) . 2 ? C6 O12 Mn1 116.9(3) . 2 ? C13 O13 Mn1 131.0(3) . . ? C22 O22 Mn3 132.4(3) . . ? C23 O23 Mn3 132.0(8) . . ? O9 C1 O1 126.0(4) . . ? O9 C1 C2 117.4(4) . . ? O1 C1 C2 116.6(4) . . ? O10 C2 O2 125.0(4) . . ? O10 C2 C1 118.6(4) . . ? O2 C2 C1 116.4(4) . . ? O7 C3 O3 125.4(4) . . ? O7 C3 C4 117.3(4) . . ? O3 C3 C4 117.3(4) . . ? O8 C4 O4 125.6(4) . . ? O8 C4 C3 118.1(4) . . ? O4 C4 C3 116.2(4) . . ? O11 C5 O5 125.5(4) . . ? O11 C5 C6 117.3(4) . . ? O5 C5 C6 117.3(4) . . ? O12 C6 O6 126.0(4) . . ? O12 C6 C5 118.0(4) . . ? O6 C6 C5 116.0(4) . . ? O13 C13 H131 109.5 . . ? O13 C13 H132 109.5 . . ? H131 C13 H132 109.5 . . ? O13 C13 H133 109.5 . . ? H131 C13 H133 109.5 . . ? H132 C13 H133 109.5 . . ? O22 C22 H221 109.5 . . ? O22 C22 H222 109.5 . . ? H221 C22 H222 109.5 . . ? O22 C22 H223 109.5 . . ? H221 C22 H223 109.5 . . ? H222 C22 H223 109.5 . . ? O23 C23 H231 109.5 . . ? O23 C23 H232 109.5 . . ? H231 C23 H232 109.5 . . ? O23 C23 H233 109.5 . . ? H231 C23 H233 109.5 . . ? H232 C23 H233 109.5 . . ? O102 O103 O102 179.997(2) 3 . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.006 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.154