# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2210 data_mnpcot _publ_contact_author_name 'Anthony K. Cheetham' _publ_contact_author_address ; Materials Research Laboratory University of California Santa Barbara CA 93106 U.S.A ; _publ_contact_author_phone '805-893 8767' _publ_contact_author_fax '805-893 8797' _publ_contact_author_email 'cheetham@mrl.ucsb.edu' _publ_requested_journal ; Journal of the Chemical Society, Dalton Transactions ; _publ_requested_coeditor_name ? _publ_section_title ; Synthesis and characterization of two manganese phosphonocarboxylates: Mn3(O3PCH2COO)2 and Mn3(O3PCH2H2COO)2 ; loop_ _publ_author_name _publ_author_address 'Stock, Norbert' ; Materials Research Laboratory University of California Santa Barbara CA 93106 U.S.A ; 'Stucky, Galen D.' ; Department of Chemistry University of California Santa Barbara CA 93106 U.S.A ; 'Cheetham, Anthony K.' ; Materials Research Laboratory University of California Santa Barbara CA 93106 U.S.A ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'manganese phosphonoacetate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 Mn3 O10 P2' _chemical_formula_weight 438.83 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3922(6) _cell_length_b 8.4863(8) _cell_length_c 10.0086(9) _cell_angle_alpha 106.1870(10) _cell_angle_beta 96.428(2) _cell_angle_gamma 101.436(2) _cell_volume 502.92(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 426 _exptl_absorpt_coefficient_mu 4.078 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5065 _exptl_absorpt_correction_T_max 0.8747 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5198 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.23 _reflns_number_total 2260 _reflns_number_gt 1978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0298P)^2^+1.0012P] 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 2260 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn -0.11513(7) 0.61494(6) 0.61207(5) 0.01774(13) Uani 1 1 d . . . Mn2 Mn -0.39985(7) 0.82792(6) 0.45075(5) 0.01760(13) Uani 1 1 d . . . Mn3 Mn 0.29834(10) 0.54859(8) 0.12154(5) 0.03103(16) Uani 1 1 d . . . P1 P 0.07882(12) 0.78399(10) 0.36467(8) 0.01353(16) Uani 1 1 d . . . P2 P 0.57454(12) 0.35714(10) 0.31617(8) 0.01437(17) Uani 1 1 d . . . O1 O -0.0794(3) 0.7782(3) 0.4679(2) 0.0160(4) Uani 1 1 d . . . O2 O 0.2971(3) 0.9065(3) 0.4397(2) 0.0184(5) Uani 1 1 d . . . O3 O 0.1140(4) 0.6105(3) 0.2882(2) 0.0191(5) Uani 1 1 d . . . O4 O -0.3137(4) 0.6559(3) 0.0507(3) 0.0296(6) Uani 1 1 d . . . O5 O -0.4191(4) 0.8093(3) 0.2336(2) 0.0236(5) Uani 1 1 d . . . O6 O 0.7891(3) 0.4105(3) 0.4201(2) 0.0159(4) Uani 1 1 d . . . O7 O 0.3934(3) 0.2701(3) 0.3784(2) 0.0201(5) Uani 1 1 d . . . O8 O 0.5074(4) 0.5035(3) 0.2796(2) 0.0236(5) Uani 1 1 d . . . O9 O 0.9966(4) 0.2509(3) 0.1751(2) 0.0258(5) Uani 1 1 d . . . O10 O 0.8261(5) 0.3362(4) 0.0156(3) 0.0369(7) Uani 1 1 d . . . C1 C -0.0377(5) 0.8669(4) 0.2325(3) 0.0190(6) Uani 1 1 d . . . H1A H -0.0352 0.9848 0.2763 0.023 Uiso 1 1 calc R . . H1B H 0.0503 0.8612 0.1592 0.023 Uiso 1 1 calc R . . C2 C -0.2685(5) 0.7703(4) 0.1660(3) 0.0191(6) Uani 1 1 d . . . C3 C 0.6123(5) 0.2059(4) 0.1590(3) 0.0233(7) Uani 1 1 d . . . H3A H 0.6126 0.0996 0.1775 0.028 Uiso 1 1 calc R . . H3B H 0.4918 0.1856 0.0833 0.028 Uiso 1 1 calc R . . C4 C 0.8246(5) 0.2675(4) 0.1116(3) 0.0214(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0150(2) 0.0200(3) 0.0181(2) 0.00419(19) 0.00212(17) 0.00663(19) Mn2 0.0135(2) 0.0233(3) 0.0192(2) 0.00933(19) 0.00397(17) 0.00704(19) Mn3 0.0417(3) 0.0457(4) 0.0139(2) 0.0079(2) 0.0049(2) 0.0310(3) P1 0.0116(4) 0.0149(4) 0.0150(3) 0.0052(3) 0.0029(3) 0.0043(3) P2 0.0125(4) 0.0191(4) 0.0132(3) 0.0065(3) 0.0024(3) 0.0055(3) O1 0.0125(10) 0.0189(11) 0.0185(10) 0.0071(8) 0.0043(8) 0.0057(8) O2 0.0116(10) 0.0180(11) 0.0246(11) 0.0052(9) 0.0023(8) 0.0036(8) O3 0.0194(11) 0.0177(11) 0.0213(11) 0.0056(9) 0.0059(9) 0.0065(9) O4 0.0316(14) 0.0303(14) 0.0211(12) 0.0002(10) -0.0035(10) 0.0100(11) O5 0.0199(12) 0.0353(14) 0.0215(11) 0.0126(10) 0.0064(9) 0.0128(10) O6 0.0126(10) 0.0171(11) 0.0172(10) 0.0047(8) 0.0006(8) 0.0039(8) O7 0.0141(11) 0.0260(12) 0.0214(11) 0.0106(9) 0.0039(8) 0.0025(9) O8 0.0254(12) 0.0256(13) 0.0243(12) 0.0124(10) 0.0008(9) 0.0114(10) O9 0.0258(12) 0.0358(15) 0.0173(11) 0.0047(10) 0.0013(9) 0.0171(11) O10 0.0428(16) 0.060(2) 0.0264(13) 0.0255(13) 0.0158(12) 0.0326(15) C1 0.0219(16) 0.0198(16) 0.0203(15) 0.0116(12) 0.0052(12) 0.0080(13) C2 0.0207(16) 0.0215(16) 0.0183(14) 0.0094(12) 0.0018(12) 0.0091(13) C3 0.0240(17) 0.0255(18) 0.0193(15) 0.0035(13) 0.0026(12) 0.0094(14) C4 0.0254(17) 0.0286(18) 0.0137(14) 0.0054(13) 0.0057(12) 0.0146(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O9 2.086(2) 2_666 ? Mn1 O6 2.130(2) 1_455 ? Mn1 O6 2.187(2) 2_666 ? Mn1 O7 2.191(2) 2_566 ? Mn1 O1 2.263(2) . ? Mn1 O3 2.393(2) 2_566 ? Mn1 Mn1 3.2315(9) 2_566 ? Mn2 O7 2.099(2) 2_566 ? Mn2 O5 2.123(2) . ? Mn2 O2 2.142(2) 2_576 ? Mn2 O1 2.170(2) . ? Mn2 O2 2.171(2) 1_455 ? Mn3 O10 2.070(3) 2_665 ? Mn3 O4 2.105(2) 2_565 ? Mn3 O8 2.122(2) . ? Mn3 O3 2.155(2) . ? Mn3 O5 2.448(3) 1_655 ? P1 O1 1.528(2) . ? P1 O3 1.531(2) . ? P1 O2 1.532(2) . ? P1 C1 1.819(3) . ? P2 O8 1.513(2) . ? P2 O6 1.530(2) . ? P2 O7 1.534(2) . ? P2 C3 1.806(3) . ? O2 Mn2 2.142(2) 2_576 ? O2 Mn2 2.171(2) 1_655 ? O3 Mn1 2.393(2) 2_566 ? O4 C2 1.244(4) . ? O4 Mn3 2.105(2) 2_565 ? O5 C2 1.281(4) . ? O5 Mn3 2.448(3) 1_455 ? O6 Mn1 2.130(2) 1_655 ? O6 Mn1 2.187(2) 2_666 ? O7 Mn2 2.099(2) 2_566 ? O7 Mn1 2.191(2) 2_566 ? O9 C4 1.260(4) . ? O9 Mn1 2.086(2) 2_666 ? O10 C4 1.255(4) . ? O10 Mn3 2.070(3) 2_665 ? C1 C2 1.512(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.530(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? 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 Mn1 O6 160.37(9) 2_666 1_455 ? O9 Mn1 O6 90.37(9) 2_666 2_666 ? O6 Mn1 O6 83.06(8) 1_455 2_666 ? O9 Mn1 O7 89.66(9) 2_666 2_566 ? O6 Mn1 O7 103.49(8) 1_455 2_566 ? O6 Mn1 O7 157.31(9) 2_666 2_566 ? O9 Mn1 O1 113.48(9) 2_666 . ? O6 Mn1 O1 84.40(8) 1_455 . ? O6 Mn1 O1 84.65(8) 2_666 . ? O7 Mn1 O1 74.58(8) 2_566 . ? O9 Mn1 O3 78.77(9) 2_666 2_566 ? O6 Mn1 O3 82.15(8) 1_455 2_566 ? O6 Mn1 O3 83.93(8) 2_666 2_566 ? O7 Mn1 O3 118.27(8) 2_566 2_566 ? O1 Mn1 O3 163.29(8) . 2_566 ? O9 Mn1 Mn1 128.69(7) 2_666 2_566 ? O6 Mn1 Mn1 42.20(6) 1_455 2_566 ? O6 Mn1 Mn1 40.86(6) 2_666 2_566 ? O7 Mn1 Mn1 141.09(6) 2_566 2_566 ? O1 Mn1 Mn1 82.68(6) . 2_566 ? O3 Mn1 Mn1 80.70(5) 2_566 2_566 ? O7 Mn2 O5 153.97(10) 2_566 . ? O7 Mn2 O2 100.68(9) 2_566 2_576 ? O5 Mn2 O2 104.73(9) . 2_576 ? O7 Mn2 O1 78.39(8) 2_566 . ? O5 Mn2 O1 93.13(8) . . ? O2 Mn2 O1 96.44(8) 2_576 . ? O7 Mn2 O2 104.23(9) 2_566 1_455 ? O5 Mn2 O2 86.82(9) . 1_455 ? O2 Mn2 O2 77.58(9) 2_576 1_455 ? O1 Mn2 O2 173.77(9) . 1_455 ? O10 Mn3 O4 90.46(11) 2_665 2_565 ? O10 Mn3 O8 161.26(12) 2_665 . ? O4 Mn3 O8 98.26(10) 2_565 . ? O10 Mn3 O3 100.51(9) 2_665 . ? O4 Mn3 O3 140.61(10) 2_565 . ? O8 Mn3 O3 83.22(9) . . ? O10 Mn3 O5 88.81(11) 2_665 1_655 ? O4 Mn3 O5 126.63(10) 2_565 1_655 ? O8 Mn3 O5 72.67(9) . 1_655 ? O3 Mn3 O5 91.61(8) . 1_655 ? O1 P1 O3 113.64(13) . . ? O1 P1 O2 110.77(12) . . ? O3 P1 O2 109.93(12) . . ? O1 P1 C1 106.69(13) . . ? O3 P1 C1 108.07(14) . . ? O2 P1 C1 107.49(14) . . ? O8 P2 O6 113.26(13) . . ? O8 P2 O7 108.47(13) . . ? O6 P2 O7 109.81(12) . . ? O8 P2 C3 110.17(15) . . ? O6 P2 C3 106.27(14) . . ? O7 P2 C3 108.79(15) . . ? P1 O1 Mn2 127.82(12) . . ? P1 O1 Mn1 127.79(12) . . ? Mn2 O1 Mn1 99.57(8) . . ? P1 O2 Mn2 134.70(13) . 2_576 ? P1 O2 Mn2 122.87(13) . 1_655 ? Mn2 O2 Mn2 102.42(9) 2_576 1_655 ? P1 O3 Mn3 127.93(13) . . ? P1 O3 Mn1 125.34(12) . 2_566 ? Mn3 O3 Mn1 102.06(9) . 2_566 ? C2 O4 Mn3 162.5(2) . 2_565 ? C2 O5 Mn2 121.48(19) . . ? C2 O5 Mn3 98.8(2) . 1_455 ? Mn2 O5 Mn3 101.70(9) . 1_455 ? P2 O6 Mn1 127.53(12) . 1_655 ? P2 O6 Mn1 131.31(12) . 2_666 ? Mn1 O6 Mn1 96.94(8) 1_655 2_666 ? P2 O7 Mn2 132.18(13) . 2_566 ? P2 O7 Mn1 113.65(13) . 2_566 ? Mn2 O7 Mn1 104.17(9) 2_566 2_566 ? P2 O8 Mn3 139.60(15) . . ? C4 O9 Mn1 121.3(2) . 2_666 ? C4 O10 Mn3 155.9(2) . 2_665 ? C2 C1 P1 112.2(2) . . ? C2 C1 H1A 109.2 . . ? P1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? O4 C2 O5 120.2(3) . . ? O4 C2 C1 122.2(3) . . ? O5 C2 C1 117.5(3) . . ? C4 C3 P2 112.0(2) . . ? C4 C3 H3A 109.2 . . ? P2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? P2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O10 C4 O9 121.7(3) . . ? O10 C4 C3 120.7(3) . . ? O9 C4 C3 117.6(3) . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 1.321 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.120 data_pct _publ_contact_author_name 'Anthony K. Cheetham' _publ_contact_author_address ; Materials Research Laboratory University of California Santa Barbara CA 93106 U.S.A ; _publ_contact_author_phone '805-893 8767' _publ_contact_author_fax '805-893 8797' _publ_contact_author_email 'cheetham@mrl.ucsb.edu' _publ_requested_journal ; Journal of the Chemical Society, Dalton Transactions ; _publ_requested_coeditor_name ? _publ_section_title ; Synthesis and characterization of two manganese phosphonocarboxylates: Mn3(O3PCH2COO)2 and Mn3(O3PCH2H2COO)2 ; loop_ _publ_author_name _publ_author_address 'Stock, Norbert' ; Materials Research Laboratory University of California Santa Barbara CA 93106 U.S.A ; 'Stucky, Galen D.' ; Department of Chemistry University of California Santa Barbara CA 93106 U.S.A ; 'Cheetham, Anthony K.' ; Materials Research Laboratory University of California Santa Barbara CA 93106 U.S.A ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'manganese phosphonopropionate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Mn3 O10 P2' _chemical_formula_weight 466.88 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.207(3) _cell_length_b 9.340(3) _cell_length_c 9.188(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.906(6) _cell_angle_gamma 90.00 _cell_volume 680.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 458 _exptl_absorpt_coefficient_mu 3.021 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2412 _exptl_absorpt_correction_T_max 0.3576 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4102 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.63 _reflns_number_total 1561 _reflns_number_gt 1124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.1319P)^2^+9.0817P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1561 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1163 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.2506 _refine_ls_wR_factor_gt 0.2329 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.0000 0.0000 0.0100(5) Uani 1 2 d S . . Mn2 Mn 0.07124(18) 0.36538(15) 0.11438(16) 0.0138(5) Uani 1 1 d . . . P1 P -0.1233(3) 0.2114(3) 0.2687(3) 0.0107(6) Uani 1 1 d . . . O1 O -0.0887(8) 0.1701(7) 0.1185(7) 0.0122(13) Uani 1 1 d . . . O2 O -0.0158(9) 0.3489(7) 0.3176(7) 0.0148(14) Uani 1 1 d . . . O3 O -0.0734(9) 0.0938(7) 0.3880(7) 0.0161(14) Uani 1 1 d . . . C1 C -0.3442(12) 0.2536(10) 0.2406(13) 0.017(2) Uani 1 1 d . . . H1A H -0.3647 0.2801 0.3364 0.021 Uiso 1 1 calc R . . H1B H -0.3722 0.3353 0.1736 0.021 Uiso 1 1 calc R . . C2 C -0.4552(13) 0.1322(12) 0.1759(15) 0.028(3) Uani 1 1 d . . . H2A H -0.4339 0.0538 0.2477 0.034 Uiso 1 1 calc R . . H2B H -0.4257 0.0995 0.0858 0.034 Uiso 1 1 calc R . . C3 C -0.6436(13) 0.1673(12) 0.1358(12) 0.021(2) Uani 1 1 d . . . O5 O -0.7444(9) 0.0654(9) 0.0919(10) 0.032(2) Uani 1 1 d . . . O6 O -0.6873(10) 0.2961(9) 0.1462(11) 0.033(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0144(10) 0.0056(10) 0.0103(9) -0.0001(7) 0.0037(7) 0.0007(7) Mn2 0.0188(8) 0.0077(7) 0.0154(8) 0.0016(5) 0.0053(6) 0.0005(5) P1 0.0121(11) 0.0075(11) 0.0124(11) -0.0004(8) 0.0030(9) 0.0001(9) O1 0.016(3) 0.013(3) 0.006(3) -0.001(2) 0.000(2) -0.003(3) O2 0.025(4) 0.005(3) 0.018(3) -0.005(2) 0.011(3) -0.001(3) O3 0.032(4) 0.003(3) 0.012(3) 0.001(2) 0.004(3) 0.007(3) C1 0.004(4) 0.015(5) 0.031(5) -0.006(4) 0.002(4) -0.001(3) C2 0.020(5) 0.014(5) 0.052(7) -0.006(5) 0.011(5) 0.005(4) C3 0.020(5) 0.013(5) 0.027(5) -0.002(4) 0.002(4) -0.009(4) O5 0.012(4) 0.025(5) 0.050(5) -0.008(4) -0.007(3) -0.007(3) O6 0.021(4) 0.018(4) 0.059(6) -0.010(4) 0.007(4) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 2.139(7) 3_455 ? Mn1 O5 2.139(7) 1_655 ? Mn1 O1 2.156(7) 3 ? Mn1 O1 2.156(7) . ? Mn1 O2 2.170(6) 2_545 ? Mn1 O2 2.170(6) 4_565 ? Mn2 O6 2.032(8) 1_655 ? Mn2 O3 2.134(7) 2 ? Mn2 O3 2.147(7) 4_565 ? Mn2 O2 2.169(7) . ? Mn2 O1 2.253(7) . ? Mn2 P1 2.791(3) . ? P1 O1 1.528(7) . ? P1 O3 1.531(7) . ? P1 O2 1.557(7) . ? P1 C1 1.808(10) . ? O2 Mn1 2.170(6) 2 ? O3 Mn2 2.134(7) 2_545 ? O3 Mn2 2.147(7) 4_566 ? C1 C2 1.480(14) . ? C2 C3 1.529(15) . ? C3 O5 1.258(12) . ? C3 O6 1.267(14) . ? O5 Mn1 2.139(7) 1_455 ? O6 Mn2 2.032(8) 1_455 ? 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 O5 180.0 3_455 1_655 ? O5 Mn1 O1 90.8(3) 3_455 3 ? O5 Mn1 O1 89.2(3) 1_655 3 ? O5 Mn1 O1 89.2(3) 3_455 . ? O5 Mn1 O1 90.8(3) 1_655 . ? O1 Mn1 O1 180.0(4) 3 . ? O5 Mn1 O2 88.7(3) 3_455 2_545 ? O5 Mn1 O2 91.3(3) 1_655 2_545 ? O1 Mn1 O2 87.1(2) 3 2_545 ? O1 Mn1 O2 92.9(2) . 2_545 ? O5 Mn1 O2 91.3(3) 3_455 4_565 ? O5 Mn1 O2 88.7(3) 1_655 4_565 ? O1 Mn1 O2 92.9(2) 3 4_565 ? O1 Mn1 O2 87.1(2) . 4_565 ? O2 Mn1 O2 180.0(3) 2_545 4_565 ? O6 Mn2 O3 108.0(3) 1_655 2 ? O6 Mn2 O3 118.1(3) 1_655 4_565 ? O3 Mn2 O3 79.4(3) 2 4_565 ? O6 Mn2 O2 112.2(3) 1_655 . ? O3 Mn2 O2 94.9(2) 2 . ? O3 Mn2 O2 128.6(3) 4_565 . ? O6 Mn2 O1 106.9(3) 1_655 . ? O3 Mn2 O1 144.7(3) 2 . ? O3 Mn2 O1 88.9(2) 4_565 . ? O2 Mn2 O1 66.8(2) . . ? O6 Mn2 P1 115.2(3) 1_655 . ? O3 Mn2 P1 121.9(2) 2 . ? O3 Mn2 P1 109.73(19) 4_565 . ? O2 Mn2 P1 33.72(18) . . ? O1 Mn2 P1 33.12(16) . . ? O1 P1 O3 112.9(4) . . ? O1 P1 O2 104.2(4) . . ? O3 P1 O2 111.0(4) . . ? O1 P1 C1 109.8(4) . . ? O3 P1 C1 109.4(5) . . ? O2 P1 C1 109.5(4) . . ? O1 P1 Mn2 53.7(3) . . ? O3 P1 Mn2 130.6(3) . . ? O2 P1 Mn2 50.7(2) . . ? C1 P1 Mn2 119.9(4) . . ? P1 O1 Mn1 143.8(4) . . ? P1 O1 Mn2 93.2(3) . . ? Mn1 O1 Mn2 108.3(3) . . ? P1 O2 Mn2 95.6(3) . . ? P1 O2 Mn1 132.5(4) . 2 ? Mn2 O2 Mn1 130.6(3) . 2 ? P1 O3 Mn2 135.3(4) . 2_545 ? P1 O3 Mn2 123.1(4) . 4_566 ? Mn2 O3 Mn2 100.6(3) 2_545 4_566 ? C2 C1 P1 112.4(7) . . ? C1 C2 C3 114.3(9) . . ? O5 C3 O6 124.5(10) . . ? O5 C3 C2 117.1(10) . . ? O6 C3 C2 118.3(9) . . ? C3 O5 Mn1 147.2(8) . 1_455 ? C3 O6 Mn2 125.2(7) . 1_455 ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 28.63 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 3.576 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.315