data_Cd(O3PCH2C6H4COOH)_H2O _publ_contact_author_name 'Norbert Stock' _publ_contact_author_address ; Ludwig-Maximilians-University Butenandtstr. 11 81377 Munich Germany ; _publ_contact_author_phone '+49-(0)89-2180-77617' _publ_contact_author_fax '+49-(0)89-2180-77622' _publ_contact_author_email 'norbert.stock@cup.uni-muenchen.de' _publ_requested_journal ; ; _publ_requested_coeditor_name ? _publ_section_title ; xxxxx ; _publ_author_name 'Stock, Norbert' _publ_author_address ; Ludwig-Maximilians-University Department of Chemistry and Biochemistry Butenandtstr. 5-13 (Haus E) 81377 Munich Germany ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H9 Cd O6 P' _chemical_formula_weight 344.52 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' '-x, -y, z+1/2' _cell_length_a 10.0229(2) _cell_length_b 5.95800(10) _cell_length_c 34.9009(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2084.16(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.258 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19947 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4635 _reflns_number_gt 3135 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+1.6735P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(11) _refine_ls_number_reflns 4635 _refine_ls_number_parameters 130 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 Cd1 Cd 0.88792(12) 0.49513(7) 0.070044(15) 0.0126(3) Uiso 1 1 d . . . Cd2 Cd 0.63812(12) 1.00090(7) 0.054611(16) 0.0124(3) Uiso 1 1 d . . . P1 P 0.6074(4) 0.4924(3) 0.01183(16) 0.0088(10) Uiso 1 1 d . . . P2 P 0.3592(4) 1.0161(3) 0.11280(18) 0.0151(11) Uiso 1 1 d . . . C1 C 0.3195(10) 0.9577(14) 0.1627(3) 0.021(2) Uiso 1 1 d . . . C2 C 0.5674(9) 0.5439(15) -0.0372(3) 0.021(2) Uiso 1 1 d . . . C3 C 0.3783(8) 1.1211(13) 0.1914(3) 0.023(2) Uiso 1 1 d . . . C4 C 0.4920(10) 1.0595(16) 0.2112(3) 0.029(2) Uiso 1 1 d . . . C5 C 0.3715(12) 1.4698(16) 0.2270(5) 0.031(3) Uiso 1 1 d . . . C6 C 0.3163(8) 1.3266(13) 0.1992(3) 0.026(2) Uiso 1 1 d . . . C7 C 0.5497(10) 1.2026(14) 0.2393(3) 0.037(2) Uiso 1 1 d . . . C8 C 0.4851(9) 1.4067(15) 0.2468(3) 0.031(2) Uiso 1 1 d . . . C9 C 0.6280(8) 0.3939(14) -0.0670(3) 0.026(2) Uiso 1 1 d . . . C10 C 0.6208(11) 0.0367(16) -0.1026(4) 0.026(3) Uiso 1 1 d . . . C11 C 0.7437(10) 0.4568(14) -0.0863(3) 0.029(2) Uiso 1 1 d . . . C12 C 0.7334(8) 0.1070(13) -0.1228(3) 0.026(2) Uiso 1 1 d . . . C13 C 0.5641(9) 0.1831(14) -0.0753(3) 0.030(2) Uiso 1 1 d . . . C14 C 0.7975(9) 0.3039(13) -0.1146(3) 0.030(2) Uiso 1 1 d . . . C15 C 0.5454(12) 1.5526(19) 0.2772(4) 0.037(3) Uiso 1 1 d . . . C16 C 0.7929(10) -0.0370(14) -0.1530(3) 0.027(2) Uiso 1 1 d . . . O1 O 0.7561(7) 0.4681(9) 0.0172(2) 0.0198(17) Uiso 1 1 d . . . O2 O 0.2828(6) 1.2283(8) 0.0993(2) 0.0167(15) Uiso 1 1 d . . . O3 O 0.2951(6) 0.8174(9) 0.0906(2) 0.0171(15) Uiso 1 1 d . . . O4 O 0.5312(6) 0.2829(9) 0.0258(2) 0.0180(16) Uiso 1 1 d . . . O5 O 0.5082(7) 1.0363(9) 0.1074(2) 0.0169(16) Uiso 1 1 d . . . O6 O 0.6607(11) 1.5053(8) 0.2900(4) 0.041(3) Uiso 1 1 d . . . O7 O 0.4717(7) 1.7249(11) 0.2862(3) 0.054(2) Uiso 1 1 d . . . O8 O 0.7216(7) -0.2219(11) -0.1617(3) 0.054(2) Uiso 1 1 d . . . O9 O 0.8931(10) 0.0009(8) -0.1700(4) 0.032(3) Uiso 1 1 d . . . O10 O 1.0506(10) 0.4922(7) 0.1192(3) 0.021(3) Uiso 1 1 d . . . O11 O 0.7958(11) 0.9852(8) 0.0052(3) 0.024(3) Uiso 1 1 d . . . O12 O 0.5447(6) 0.6900(9) 0.0336(2) 0.0180(16) Uiso 1 1 d . . . _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 Cd1 O3 2.202(6) 3_565 ? Cd1 O2 2.206(6) 3_575 ? Cd1 O1 2.275(8) . ? Cd1 O12 2.303(7) 3_565 ? Cd1 O10 2.367(11) . ? Cd1 O4 2.489(6) 3_565 ? Cd1 P1 2.996(5) 3_565 ? Cd2 O12 2.202(6) . ? Cd2 O4 2.232(6) 1_565 ? Cd2 O5 2.267(8) . ? Cd2 O3 2.286(6) 3_575 ? Cd2 O11 2.340(12) . ? Cd2 O2 2.529(6) 3_575 ? Cd2 P2 3.007(6) 3_575 ? P1 O1 1.508(8) . ? P1 O12 1.536(7) . ? P1 O4 1.542(6) . ? P1 C2 1.784(12) . ? P1 Cd1 2.996(5) 3_465 ? P2 O5 1.510(8) . ? P2 O3 1.553(7) . ? P2 O2 1.552(6) . ? P2 C1 1.820(12) . ? P2 Cd2 3.007(5) 3_475 ? C1 C3 1.516(13) . ? C2 C9 1.500(14) . ? C3 C4 1.382(12) . ? C3 C6 1.400(11) . ? C4 C7 1.421(12) . ? C5 C8 1.385(15) . ? C5 C6 1.407(15) . ? C7 C8 1.403(12) . ? C8 C15 1.497(15) . ? C9 C11 1.393(13) . ? C9 C13 1.440(12) . ? C10 C12 1.395(14) . ? C10 C13 1.410(14) . ? C11 C14 1.448(12) . ? C12 C14 1.368(11) . ? C12 C16 1.485(13) . ? C15 O6 1.270(17) . ? C15 O7 1.303(12) . ? C16 O9 1.187(15) . ? C16 O8 1.348(10) . ? O2 Cd1 2.206(6) 3_475 ? O2 Cd2 2.529(6) 3_475 ? O3 Cd1 2.202(6) 3_465 ? O3 Cd2 2.286(6) 3_475 ? O4 Cd2 2.232(6) 1_545 ? O4 Cd1 2.489(6) 3_465 ? O12 Cd1 2.303(7) 3_465 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O2 106.2(2) 3_565 3_575 ? O3 Cd1 O1 87.7(2) 3_565 . ? O2 Cd1 O1 98.6(2) 3_575 . ? O3 Cd1 O12 93.6(2) 3_565 3_565 ? O2 Cd1 O12 159.9(2) 3_575 3_565 ? O1 Cd1 O12 85.1(3) . 3_565 ? O3 Cd1 O10 92.8(3) 3_565 . ? O2 Cd1 O10 90.0(3) 3_575 . ? O1 Cd1 O10 170.9(3) . . ? O12 Cd1 O10 85.8(3) 3_565 . ? O3 Cd1 O4 153.6(3) 3_565 3_565 ? O2 Cd1 O4 99.5(2) 3_575 3_565 ? O1 Cd1 O4 82.5(3) . 3_565 ? O12 Cd1 O4 61.2(2) 3_565 3_565 ? O10 Cd1 O4 93.2(3) . 3_565 ? O3 Cd1 P1 123.55(18) 3_565 3_565 ? O2 Cd1 P1 130.23(16) 3_575 3_565 ? O1 Cd1 P1 83.0(2) . 3_565 ? O12 Cd1 P1 30.25(15) 3_565 3_565 ? O10 Cd1 P1 89.2(3) . 3_565 ? O4 Cd1 P1 30.94(14) 3_565 3_565 ? O12 Cd2 O4 106.2(3) . 1_565 ? O12 Cd2 O5 96.0(2) . . ? O4 Cd2 O5 91.2(2) 1_565 . ? O12 Cd2 O3 151.0(2) . 3_575 ? O4 Cd2 O3 102.8(2) 1_565 3_575 ? O5 Cd2 O3 84.5(3) . 3_575 ? O12 Cd2 O11 90.5(3) . . ? O4 Cd2 O11 91.3(3) 1_565 . ? O5 Cd2 O11 172.1(3) . . ? O3 Cd2 O11 87.7(3) 3_575 . ? O12 Cd2 O2 89.7(2) . 3_575 ? O4 Cd2 O2 163.6(2) 1_565 3_575 ? O5 Cd2 O2 83.0(3) . 3_575 ? O3 Cd2 O2 61.5(2) 3_575 3_575 ? O11 Cd2 O2 92.6(3) . 3_575 ? O12 Cd2 P2 120.68(18) . 3_575 ? O4 Cd2 P2 133.08(16) 1_565 3_575 ? O5 Cd2 P2 82.9(2) . 3_575 ? O3 Cd2 P2 30.41(16) 3_575 3_575 ? O11 Cd2 P2 89.9(3) . 3_575 ? O2 Cd2 P2 31.05(14) 3_575 3_575 ? O1 P1 O12 114.6(4) . . ? O1 P1 O4 111.8(4) . . ? O12 P1 O4 105.1(5) . . ? O1 P1 C2 111.0(5) . . ? O12 P1 C2 104.5(4) . . ? O4 P1 C2 109.3(4) . . ? O1 P1 Cd1 130.1(4) . 3_465 ? O12 P1 Cd1 49.1(3) . 3_465 ? O4 P1 Cd1 56.1(3) . 3_465 ? C2 P1 Cd1 118.7(4) . 3_465 ? O5 P2 O3 114.1(4) . . ? O5 P2 O2 112.6(4) . . ? O3 P2 O2 105.4(5) . . ? O5 P2 C1 110.5(5) . . ? O3 P2 C1 104.0(4) . . ? O2 P2 C1 109.8(5) . . ? O5 P2 Cd2 130.3(4) . 3_475 ? O3 P2 Cd2 48.2(3) . 3_475 ? O2 P2 Cd2 57.2(3) . 3_475 ? C1 P2 Cd2 118.6(4) . 3_475 ? C3 C1 P2 115.2(7) . . ? C9 C2 P1 118.1(7) . . ? C4 C3 C6 120.1(8) . . ? C4 C3 C1 118.7(8) . . ? C6 C3 C1 121.1(8) . . ? C3 C4 C7 121.3(9) . . ? C8 C5 C6 120.3(9) . . ? C3 C6 C5 119.3(8) . . ? C8 C7 C4 117.6(9) . . ? C5 C8 C7 121.4(9) . . ? C5 C8 C15 121.9(9) . . ? C7 C8 C15 116.8(9) . . ? C11 C9 C13 120.5(9) . . ? C11 C9 C2 120.9(8) . . ? C13 C9 C2 118.7(8) . . ? C12 C10 C13 118.8(9) . . ? C9 C11 C14 118.1(8) . . ? C14 C12 C10 122.1(9) . . ? C14 C12 C16 117.1(8) . . ? C10 C12 C16 120.7(8) . . ? C10 C13 C9 119.8(9) . . ? C12 C14 C11 120.5(9) . . ? O6 C15 O7 127.3(11) . . ? O6 C15 C8 119.2(10) . . ? O7 C15 C8 113.5(10) . . ? O9 C16 O8 119.4(10) . . ? O9 C16 C12 125.8(9) . . ? O8 C16 C12 114.8(9) . . ? P1 O1 Cd1 131.9(5) . . ? P2 O2 Cd1 120.9(4) . 3_475 ? P2 O2 Cd2 91.8(3) . 3_475 ? Cd1 O2 Cd2 113.1(3) 3_475 3_475 ? P2 O3 Cd1 129.2(4) . 3_465 ? P2 O3 Cd2 101.4(3) . 3_475 ? Cd1 O3 Cd2 120.8(3) 3_465 3_475 ? P1 O4 Cd2 120.9(4) . 1_545 ? P1 O4 Cd1 93.0(3) . 3_465 ? Cd2 O4 Cd1 113.4(3) 1_545 3_465 ? P2 O5 Cd2 131.4(5) . . ? P1 O12 Cd2 129.5(4) . . ? P1 O12 Cd1 100.7(3) . 3_465 ? Cd2 O12 Cd1 120.6(3) . 3_465 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.527 _refine_diff_density_min -2.568 _refine_diff_density_rms 0.207 data_Cu(HO3PCH2C6H4COOH)2_2H2O _publ_contact_author_name 'Norbert Stock' _publ_contact_author_address ; Ludwig-Maximilians-University Butenandtstr. 11 81377 Munich Germany ; _publ_contact_author_phone '+49-(0)89-2180-77617' _publ_contact_author_fax '+49-(0)89-2180-77622' _publ_contact_author_email 'norbert.stock@cup.uni-muenchen.de' _publ_requested_journal ; ; _publ_requested_coeditor_name ? _publ_section_title ; xxxxx ; _publ_author_name 'Stock, Norbert' _publ_author_address ; Ludwig-Maximilians-University Department of Chemistry and Biochemistry Butenandtstr. 5-13 (Haus E) 81377 Munich Germany ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;Copper di(4-methylene-hydrogenphosphono-benzoic acid)-di-hydrate ; _chemical_formula_moiety 'Cu 2+, 2(HO3PCH2C6H4COOH)-, 2H2 O' _chemical_formula_sum 'C16 H20 Cu O12 P2' _chemical_formula_weight 529.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'O' 'O' 0.0106 0.0060 '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' _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 4.5914(6) _cell_length_b 5.9810(8) _cell_length_c 17.811(3) _cell_angle_alpha 81.513(16) _cell_angle_beta 86.272(16) _cell_angle_gamma 82.251(15) _cell_volume 478.82(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour white _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 271 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8988 _exptl_absorpt_correction_T_max 0.9861 _exptl_absorpt_process_details 'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)' _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 'Stoe IPDS' _diffrn_measurement_method 'area detection' diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4646 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.1498 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.99 _reflns_number_total 2127 _reflns_number_gt 1234 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0132(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2127 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.809 _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 Cu1 Cu 1.5000 0.5000 0.5000 0.0080(2) Uani 1 2 d S . . P1 P 1.0064(2) 0.34132(15) 0.38554(5) 0.0068(3) Uani 1 1 d . . . O1 O 0.8153(6) 0.5279(4) 0.42088(14) 0.0089(6) Uani 1 1 d . . . O2 O 1.2743(5) 0.2304(4) 0.42975(14) 0.0089(6) Uani 1 1 d . . . O3 O 0.8193(6) 0.1496(5) 0.37354(18) 0.0154(7) Uani 1 1 d . . . H31 H 0.692(11) 0.169(9) 0.384(3) 0.018 Uiso 1 1 d . . . O4 O 0.1853(7) 1.0703(5) 0.06959(18) 0.0279(9) Uani 1 1 d . . . O5 O 0.2040(7) 0.7325(5) 0.02854(18) 0.0261(9) Uani 1 1 d . . . H51 H 0.123(12) 0.792(9) 0.000(3) 0.031 Uiso 1 1 d . . . O6 O 1.2689(6) 0.7660(6) 0.4427(2) 0.0151(8) Uani 1 1 d . . . H61 H 1.295(11) 0.902(8) 0.444(3) 0.018 Uiso 1 1 d . . . H62 H 1.152(12) 0.759(10) 0.440(3) 0.018 Uiso 1 1 d . . . C1 C 1.1436(9) 0.4564(6) 0.2930(2) 0.0120(9) Uani 1 1 d . . . H1B H 1.2659 0.5722 0.2991 0.014 Uiso 1 1 calc R . . H1A H 1.2685 0.3356 0.2714 0.014 Uiso 1 1 calc R . . C2 C 0.9113(9) 0.5607(6) 0.2368(2) 0.0121(9) Uani 1 1 d . . . C3 C 0.8338(9) 0.4371(7) 0.1829(2) 0.0154(9) Uani 1 1 d . . . H3A H 0.9218 0.2878 0.1826 0.018 Uiso 1 1 calc R . . C4 C 0.6272(9) 0.5308(6) 0.1292(2) 0.0146(9) Uani 1 1 d . . . H4A H 0.5774 0.4454 0.0935 0.018 Uiso 1 1 calc R . . C5 C 0.4963(9) 0.7557(6) 0.1302(2) 0.0125(9) Uani 1 1 d . . . C6 C 0.5727(9) 0.8803(6) 0.1843(2) 0.0140(9) Uani 1 1 d . . . H6A H 0.4859 1.0299 0.1846 0.017 Uiso 1 1 calc R . . C7 C 0.7755(9) 0.7846(6) 0.2375(2) 0.0155(9) Uani 1 1 d . . . H7A H 0.8221 0.8690 0.2739 0.019 Uiso 1 1 calc R . . C8 C 0.2808(9) 0.8640(7) 0.0727(2) 0.0156(9) 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 Cu1 0.0070(5) 0.0074(4) 0.0078(5) 0.0019(3) 0.0007(3) 0.0021(4) P1 0.0043(6) 0.0075(5) 0.0083(6) -0.0003(4) -0.0019(4) 0.0001(5) O1 0.0056(14) 0.0089(12) 0.0113(13) -0.0005(10) -0.0002(11) 0.0014(11) O2 0.0063(14) 0.0095(12) 0.0108(14) -0.0005(10) -0.0031(11) -0.0008(11) O3 0.0068(16) 0.0174(14) 0.0236(17) -0.0064(12) -0.0004(14) -0.0038(14) O4 0.032(2) 0.0194(15) 0.031(2) -0.0009(14) -0.0168(16) 0.0064(16) O5 0.027(2) 0.0322(19) 0.0188(18) -0.0040(14) -0.0157(15) 0.0046(16) O6 0.0080(17) 0.0087(13) 0.0274(17) 0.0036(12) -0.0062(15) -0.0003(15) C1 0.009(2) 0.0176(19) 0.0102(19) -0.0007(15) 0.0014(16) -0.0050(17) C2 0.010(2) 0.019(2) 0.0059(18) 0.0051(15) 0.0011(15) -0.0026(17) C3 0.015(2) 0.0148(19) 0.015(2) -0.0018(16) -0.0031(17) 0.0052(18) C4 0.013(2) 0.021(2) 0.011(2) -0.0064(16) -0.0018(16) -0.0015(18) C5 0.009(2) 0.0177(19) 0.009(2) 0.0037(16) -0.0017(16) -0.0041(17) C6 0.018(2) 0.0093(18) 0.013(2) 0.0009(15) -0.0012(18) 0.0004(18) C7 0.018(2) 0.018(2) 0.012(2) -0.0044(16) -0.0026(17) -0.0052(18) C8 0.015(2) 0.024(2) 0.008(2) -0.0005(17) 0.0017(17) -0.0054(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 Cu1 O1 1.960(2) 1_655 ? Cu1 O1 1.960(2) 2_766 ? Cu1 O6 1.976(3) 2_866 ? Cu1 O6 1.976(3) . ? P1 O1 1.511(2) . ? P1 O2 1.525(3) . ? P1 O3 1.569(4) . ? P1 C1 1.798(4) . ? O1 Cu1 1.960(2) 1_455 ? O4 C8 1.247(5) . ? O5 C8 1.287(5) . ? C1 C2 1.518(5) . ? C2 C3 1.385(6) . ? C2 C7 1.400(5) . ? C3 C4 1.395(6) . ? C4 C5 1.399(5) . ? C5 C6 1.390(6) . ? C5 C8 1.486(5) . ? C6 C7 1.380(6) . ? 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 Cu1 O1 180.000(1) 1_655 2_766 ? O1 Cu1 O6 91.48(11) 1_655 2_866 ? O1 Cu1 O6 88.52(11) 2_766 2_866 ? O1 Cu1 O6 88.52(11) 1_655 . ? O1 Cu1 O6 91.48(11) 2_766 . ? O6 Cu1 O6 180.00(19) 2_866 . ? O1 P1 O2 115.37(15) . . ? O1 P1 O3 110.19(15) . . ? O2 P1 O3 108.30(15) . . ? O1 P1 C1 109.26(16) . . ? O2 P1 C1 106.53(16) . . ? O3 P1 C1 106.81(18) . . ? P1 O1 Cu1 128.67(15) . 1_455 ? C2 C1 P1 115.6(3) . . ? C3 C2 C7 118.8(3) . . ? C3 C2 C1 120.5(3) . . ? C7 C2 C1 120.8(4) . . ? C2 C3 C4 121.7(3) . . ? C3 C4 C5 118.7(4) . . ? C6 C5 C4 119.8(3) . . ? C6 C5 C8 119.7(3) . . ? C4 C5 C8 120.4(4) . . ? C7 C6 C5 120.8(3) . . ? C6 C7 C2 120.2(4) . . ? O4 C8 O5 124.0(4) . . ? O4 C8 C5 120.1(4) . . ? O5 C8 C5 116.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Cu1 -83.9(2) . . . 1_455 ? O3 P1 O1 Cu1 39.1(2) . . . 1_455 ? C1 P1 O1 Cu1 156.1(2) . . . 1_455 ? O1 P1 C1 C2 -59.1(3) . . . . ? O2 P1 C1 C2 175.6(3) . . . . ? O3 P1 C1 C2 60.0(3) . . . . ? P1 C1 C2 C3 -98.5(4) . . . . ? P1 C1 C2 C7 82.7(4) . . . . ? C7 C2 C3 C4 0.7(6) . . . . ? C1 C2 C3 C4 -178.2(4) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? C3 C4 C5 C8 178.4(4) . . . . ? C4 C5 C6 C7 -0.3(6) . . . . ? C8 C5 C6 C7 -179.0(4) . . . . ? C5 C6 C7 C2 1.1(6) . . . . ? C3 C2 C7 C6 -1.2(6) . . . . ? C1 C2 C7 C6 177.6(4) . . . . ? C6 C5 C8 O4 5.2(6) . . . . ? C4 C5 C8 O4 -173.5(4) . . . . ? C6 C5 C8 O5 -174.7(4) . . . . ? C4 C5 C8 O5 6.6(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H31 O2 0.60(5) 2.04(5) 2.643(4) 175(7) 1_455 O5 H51 O4 0.68(5) 1.96(5) 2.621(4) 167(7) 2_575 O6 H61 O2 0.84(5) 1.93(5) 2.756(4) 166(5) 1_565 O6 H62 O1 0.55(6) 2.28(6) 2.754(5) 146(7) . _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.428 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.112 data_Mn(HO3PCH2C6H4COOH)2_2H2O _publ_contact_author_name 'Norbert Stock' _publ_contact_author_address ; Ludwig-Maximilians-University Butenandtstr. 11 81377 Munich Germany ; _publ_contact_author_phone '+49-(0)89-2180-77617' _publ_contact_author_fax '+49-(0)89-2180-77622' _publ_contact_author_email 'norbert.stock@cup.uni-muenchen.de' _publ_requested_journal ; ; _publ_requested_coeditor_name ? _publ_section_title ; xxxxx ; _publ_author_name 'Stock, Norbert' _publ_author_address ; Ludwig-Maximilians-University Deoartment of Chemistry and Biochemistry Butenandtstr. 5-13 (Haus E) 81377 Munich Germany ; _audit_creation_method SHELXL-97 _chemical_name_systematic ;Manganese di(4-methylene-hydrogenphosphono-benzoic acid)-di-hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Mn2+, 2(HO3PCH2C6H4COOH)-, 2H2O' _chemical_formula_sum 'C16 H20 Mn O12 P2' _chemical_formula_weight 521.20 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' 'P' 'P' 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.61980(10) _cell_length_b 5.9379(2) _cell_length_c 18.0676(2) _cell_angle_alpha 83.119(2) _cell_angle_beta 88.307(2) _cell_angle_gamma 84.461(2) _cell_volume 489.68(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description stick _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 267 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.7732 _exptl_absorpt_correction_T_max 0.9373 _exptl_absorpt_process_details 'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _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 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'vertically mounted graphite crystal' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9266 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.38 _reflns_number_total 2181 _reflns_number_gt 1771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+0.3064P] 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 0.010(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2181 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.5000 0.5000 0.01473(15) Uani 1 2 d S . . P1 P 0.47415(11) 0.61071(9) 0.62130(3) 0.01426(16) Uani 1 1 d . . . O1 O 0.2036(3) 0.7092(3) 0.57768(8) 0.0165(3) Uani 1 1 d . . . O2 O 0.6689(3) 0.4360(2) 0.58434(8) 0.0168(3) Uani 1 1 d . . . O3 O 0.6557(3) 0.8134(3) 0.63616(9) 0.0199(4) Uani 1 1 d . . . H3 H 0.813(6) 0.800(5) 0.6195(15) 0.024 Uiso 1 1 d . . . O4 O 1.3206(4) -0.0771(3) 0.92766(10) 0.0368(5) Uani 1 1 d . . . H4 H 1.4384 -0.1482 0.9655 0.044 Uiso 1 1 d R . . O5 O 1.2840(4) 0.2536(3) 0.97585(10) 0.0365(5) Uani 1 1 d . . . O6 O -0.2496(4) 0.8163(3) 0.45782(10) 0.0245(4) Uani 1 1 d . . . H61 H -0.226(6) 0.949(5) 0.4498(15) 0.029 Uiso 1 1 d . . . H62 H -0.412(7) 0.804(5) 0.4420(15) 0.029 Uiso 1 1 d . . . C1 C 0.3458(5) 0.4943(4) 0.71143(12) 0.0205(5) Uani 1 1 d . . . H1B H 0.2221 0.6125 0.7327 0.025 Uiso 1 1 calc R . . H1A H 0.2259 0.3733 0.7046 0.025 Uiso 1 1 calc R . . C2 C 0.5766(5) 0.4005(4) 0.76702(11) 0.0182(5) Uani 1 1 d . . . C3 C 0.7128(5) 0.1808(4) 0.76583(13) 0.0238(5) Uani 1 1 d . . . H3A H 0.6647 0.0930 0.7295 0.029 Uiso 1 1 calc R . . C4 C 0.9184(5) 0.0923(4) 0.81806(13) 0.0239(5) Uani 1 1 d . . . H4A H 1.0064 -0.0549 0.8169 0.029 Uiso 1 1 calc R . . C5 C 0.9946(5) 0.2224(4) 0.87238(12) 0.0202(5) Uani 1 1 d . . . C6 C 0.8616(5) 0.4420(4) 0.87377(13) 0.0236(5) Uani 1 1 d . . . H6A H 0.9118 0.5303 0.9097 0.028 Uiso 1 1 calc R . . C7 C 0.6545(5) 0.5290(4) 0.82154(13) 0.0232(5) Uani 1 1 d . . . H7A H 0.5657 0.6759 0.8229 0.028 Uiso 1 1 calc R . . C8 C 1.2130(5) 0.1252(4) 0.92861(12) 0.0218(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0127(2) 0.0149(3) 0.0163(2) -0.00143(17) -0.00048(17) -0.00064(17) P1 0.0119(3) 0.0159(3) 0.0151(3) -0.0019(2) -0.0016(2) -0.0016(2) O1 0.0134(7) 0.0163(8) 0.0198(8) -0.0022(6) -0.0030(6) -0.0001(6) O2 0.0146(7) 0.0169(8) 0.0193(8) -0.0042(6) 0.0003(6) -0.0018(6) O3 0.0141(8) 0.0208(8) 0.0265(9) -0.0081(6) -0.0005(7) -0.0037(6) O4 0.0393(11) 0.0331(11) 0.0358(10) -0.0003(8) -0.0177(8) 0.0081(9) O5 0.0361(11) 0.0438(12) 0.0295(10) -0.0105(8) -0.0141(8) 0.0079(9) O6 0.0188(8) 0.0158(8) 0.0383(10) 0.0013(7) -0.0095(7) -0.0020(7) C1 0.0159(11) 0.0263(12) 0.0184(11) 0.0002(9) -0.0003(9) -0.0005(9) C2 0.0149(11) 0.0246(12) 0.0149(10) 0.0002(9) 0.0013(8) -0.0036(9) C3 0.0259(12) 0.0247(13) 0.0219(11) -0.0044(9) -0.0037(10) -0.0049(10) C4 0.0248(12) 0.0213(12) 0.0250(12) -0.0016(9) -0.0022(10) -0.0003(9) C5 0.0178(11) 0.0257(12) 0.0167(11) -0.0001(9) -0.0007(9) -0.0031(9) C6 0.0242(12) 0.0281(13) 0.0195(11) -0.0069(9) -0.0038(9) -0.0010(10) C7 0.0240(12) 0.0207(12) 0.0242(12) -0.0041(9) -0.0009(10) 0.0027(9) C8 0.0197(11) 0.0273(13) 0.0175(11) -0.0001(9) -0.0008(9) -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 Mn1 O2 2.1546(14) 1_455 ? Mn1 O2 2.1546(14) 2_666 ? Mn1 O6 2.1746(17) 2_566 ? Mn1 O6 2.1746(17) . ? Mn1 O1 2.2628(15) . ? Mn1 O1 2.2628(15) 2_566 ? P1 O2 1.5105(15) . ? P1 O1 1.5270(15) . ? P1 O3 1.5843(16) . ? P1 C1 1.798(2) . ? O2 Mn1 2.1546(14) 1_655 ? O4 C8 1.257(3) . ? O5 C8 1.280(3) . ? C1 C2 1.507(3) . ? C2 C7 1.392(3) . ? C2 C3 1.395(3) . ? C3 C4 1.381(3) . ? C4 C5 1.392(3) . ? C5 C6 1.390(3) . ? C5 C8 1.480(3) . ? C6 C7 1.384(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 O2 180.000(1) 1_455 2_666 ? O2 Mn1 O6 90.18(6) 1_455 2_566 ? O2 Mn1 O6 89.82(6) 2_666 2_566 ? O2 Mn1 O6 89.82(6) 1_455 . ? O2 Mn1 O6 90.18(6) 2_666 . ? O6 Mn1 O6 180.00(9) 2_566 . ? O2 Mn1 O1 88.22(5) 1_455 . ? O2 Mn1 O1 91.78(5) 2_666 . ? O6 Mn1 O1 94.01(6) 2_566 . ? O6 Mn1 O1 85.99(6) . . ? O2 Mn1 O1 91.78(5) 1_455 2_566 ? O2 Mn1 O1 88.22(5) 2_666 2_566 ? O6 Mn1 O1 85.99(6) 2_566 2_566 ? O6 Mn1 O1 94.01(6) . 2_566 ? O1 Mn1 O1 180.0 . 2_566 ? O2 P1 O1 114.98(8) . . ? O2 P1 O3 109.33(9) . . ? O1 P1 O3 108.75(9) . . ? O2 P1 C1 111.52(10) . . ? O1 P1 C1 106.15(9) . . ? O3 P1 C1 105.66(10) . . ? P1 O1 Mn1 120.32(8) . . ? P1 O2 Mn1 127.20(9) . 1_655 ? C2 C1 P1 116.07(15) . . ? C7 C2 C3 118.5(2) . . ? C7 C2 C1 120.8(2) . . ? C3 C2 C1 120.6(2) . . ? C4 C3 C2 120.7(2) . . ? C3 C4 C5 120.3(2) . . ? C6 C5 C4 119.5(2) . . ? C6 C5 C8 120.6(2) . . ? C4 C5 C8 119.9(2) . . ? C7 C6 C5 119.9(2) . . ? C6 C7 C2 121.1(2) . . ? O4 C8 O5 123.2(2) . . ? O4 C8 C5 119.0(2) . . ? O5 C8 C5 117.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Mn1 28.51(12) . . . . ? O3 P1 O1 Mn1 151.45(9) . . . . ? C1 P1 O1 Mn1 -95.28(11) . . . . ? O2 Mn1 O1 P1 102.65(10) 1_455 . . . ? O2 Mn1 O1 P1 -77.35(10) 2_666 . . . ? O6 Mn1 O1 P1 12.60(10) 2_566 . . . ? O6 Mn1 O1 P1 -167.40(10) . . . . ? O1 Mn1 O1 P1 -101(100) 2_566 . . . ? O1 P1 O2 Mn1 83.48(12) . . . 1_655 ? O3 P1 O2 Mn1 -39.15(13) . . . 1_655 ? C1 P1 O2 Mn1 -155.62(11) . . . 1_655 ? O2 P1 C1 C2 58.2(2) . . . . ? O1 P1 C1 C2 -175.91(16) . . . . ? O3 P1 C1 C2 -60.53(19) . . . . ? P1 C1 C2 C7 98.9(2) . . . . ? P1 C1 C2 C3 -82.4(2) . . . . ? C7 C2 C3 C4 0.6(3) . . . . ? C1 C2 C3 C4 -178.1(2) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? C3 C4 C5 C8 179.4(2) . . . . ? C4 C5 C6 C7 0.3(3) . . . . ? C8 C5 C6 C7 -179.0(2) . . . . ? C5 C6 C7 C2 -0.3(3) . . . . ? C3 C2 C7 C6 -0.2(3) . . . . ? C1 C2 C7 C6 178.5(2) . . . . ? C6 C5 C8 O4 177.2(2) . . . . ? C4 C5 C8 O4 -2.1(3) . . . . ? C6 C5 C8 O5 -3.2(3) . . . . ? C4 C5 C8 O5 177.5(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O1 0.78(3) 1.99(3) 2.757(2) 170(3) 1_655 O6 H61 O1 0.80(3) 2.04(3) 2.841(2) 174(3) 2_576 O6 H62 O2 0.82(3) 2.05(3) 2.738(2) 142(3) 2_566 O4 H4 O5 0.92 1.71 2.618(2) 167.5 2_857 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.38 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.413 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.130 data_Mn(O3PCH2C6H4COOH)_H2O _publ_contact_author_name 'Norbert Stock' _publ_contact_author_address ; Ludwig-Maximilians-University Butenandtstr. 11 81377 Munich Germany ; _publ_contact_author_phone '+49-(0)89-2180-77617' _publ_contact_author_fax '+49-(0)89-2180-77622' _publ_contact_author_email 'norbert.stock@cup.uni-muenchen.de' _publ_requested_journal ; ; _publ_requested_coeditor_name ? _publ_section_title ; xxxxx ; _publ_author_name 'Stock, Norbert' _publ_author_address ; Ludwig-Maximilians-University Department of Chemistry and Biochemistry Butenandtstr. 5-13 (Haus E) 81377 Munich Germany ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H9 Mn O6 P' _chemical_formula_weight 287.06 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' 'P' 'P' 0.1023 0.0942 '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' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' '-x, -y, z+1/2' _cell_length_a 9.82610(10) _cell_length_b 5.83930(10) _cell_length_c 35.2520(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2022.67(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.472 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23964 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4626 _reflns_number_gt 3053 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+6.6247P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(8) _refine_ls_number_reflns 4626 _refine_ls_number_parameters 130 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.2288 _refine_ls_wR_factor_gt 0.2050 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 0.90178(19) 0.49337(17) 0.06871(4) 0.0141(5) Uiso 1 1 d . . . Mn2 Mn 0.65115(17) 1.00056(17) 0.05564(3) 0.0110(4) Uiso 1 1 d . . . P1 P 0.6230(3) 0.4968(3) 0.01418(9) 0.0080(6) Uiso 1 1 d . . . P2 P 0.3734(4) 1.0099(3) 0.10998(10) 0.0149(7) Uiso 1 1 d . . . C1 C 0.3290(9) 0.9694(13) 0.1593(3) 0.017(2) Uiso 1 1 d . . . C2 C 0.5796(11) 0.5482(19) -0.0354(3) 0.031(2) Uiso 1 1 d . . . C3 C 0.3872(9) 1.1183(16) 0.1886(3) 0.027(2) Uiso 1 1 d . . . C4 C 0.5035(11) 1.0455(18) 0.2087(3) 0.028(2) Uiso 1 1 d . . . C5 C 0.3677(15) 1.4751(18) 0.2253(5) 0.045(4) Uiso 1 1 d . . . C6 C 0.3245(9) 1.3282(16) 0.1965(3) 0.027(2) Uiso 1 1 d . . . C7 C 0.5556(10) 1.1897(16) 0.2372(3) 0.037(2) Uiso 1 1 d . . . C8 C 0.4890(10) 1.4063(17) 0.2457(3) 0.032(2) Uiso 1 1 d . . . C9 C 0.6371(9) 0.3874(16) -0.0637(3) 0.026(2) Uiso 1 1 d . . . C10 C 0.6294(10) 0.0270(14) -0.1006(3) 0.019(2) Uiso 1 1 d . . . C11 C 0.7525(12) 0.4568(19) -0.0848(3) 0.037(3) Uiso 1 1 d . . . C12 C 0.7411(10) 0.1054(17) -0.1208(3) 0.036(2) Uiso 1 1 d . . . C13 C 0.5727(10) 0.1804(18) -0.0723(3) 0.035(2) Uiso 1 1 d . . . C14 C 0.8057(10) 0.3096(16) -0.1129(3) 0.033(2) Uiso 1 1 d . . . C15 C 0.5443(12) 1.5424(19) 0.2762(3) 0.033(3) Uiso 1 1 d . . . C16 C 0.7986(13) -0.0375(19) -0.1515(4) 0.038(3) Uiso 1 1 d . . . O1 O 0.7733(9) 0.4819(10) 0.0185(3) 0.025(2) Uiso 1 1 d . . . O2 O 0.3000(6) 1.2259(9) 0.09560(16) 0.0141(14) Uiso 1 1 d . . . O3 O 0.3066(6) 0.8045(10) 0.08987(18) 0.0179(15) Uiso 1 1 d . . . O4 O 0.5495(7) 0.2856(11) 0.03030(18) 0.0218(17) Uiso 1 1 d . . . O5 O 0.5275(7) 1.0199(8) 0.1049(2) 0.0128(17) Uiso 1 1 d . . . O6 O 0.6420(9) 1.5019(10) 0.2930(3) 0.039(2) Uiso 1 1 d . . . O7 O 0.4759(8) 1.7251(15) 0.2855(3) 0.064(2) Uiso 1 1 d . . . O8 O 0.7247(8) -0.2228(13) -0.1601(3) 0.056(2) Uiso 1 1 d . . . O9 O 0.9180(8) 0.0020(9) -0.1658(3) 0.028(2) Uiso 1 1 d . . . O10 O 1.0609(9) 0.4956(8) 0.1157(3) 0.022(2) Uiso 1 1 d . . . O11 O 0.7996(8) 0.9906(8) 0.0079(3) 0.019(2) Uiso 1 1 d . . . O12 O 0.5569(6) 0.6991(10) 0.03621(18) 0.0167(14) Uiso 1 1 d . . . _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3 2.111(6) 3_565 ? Mn1 O2 2.141(6) 3_575 ? Mn1 O1 2.174(10) . ? Mn1 O12 2.214(6) 3_565 ? Mn1 O10 2.277(10) . ? Mn1 O4 2.368(7) 3_565 ? Mn1 P1 2.903(4) 3_565 ? Mn2 O12 2.103(6) . ? Mn2 O5 2.123(8) . ? Mn2 O4 2.137(7) 1_565 ? Mn2 O11 2.229(9) . ? Mn2 O3 2.255(6) 3_575 ? Mn2 O2 2.423(6) 3_575 ? Mn2 P2 2.905(4) 3_575 ? P1 O1 1.487(9) . ? P1 O4 1.538(7) . ? P1 O12 1.556(7) . ? P1 C2 1.823(13) . ? P1 Mn1 2.903(4) 3_465 ? P2 O5 1.526(8) . ? P2 O3 1.540(7) . ? P2 O2 1.539(6) . ? P2 C1 1.809(11) . ? P2 Mn2 2.905(4) 3_475 ? C1 C3 1.466(13) . ? C2 C9 1.483(15) . ? C3 C6 1.399(13) . ? C3 C4 1.409(14) . ? C4 C7 1.409(14) . ? C5 C6 1.396(17) . ? C5 C8 1.448(17) . ? C7 C8 1.455(13) . ? C8 C15 1.444(15) . ? C9 C13 1.398(13) . ? C9 C11 1.414(15) . ? C10 C12 1.386(14) . ? C10 C13 1.452(14) . ? C11 C14 1.413(14) . ? C12 C14 1.379(13) . ? C12 C16 1.477(16) . ? C15 O6 1.154(15) . ? C15 O7 1.302(12) . ? C16 O9 1.299(15) . ? C16 O8 1.338(12) . ? O2 Mn1 2.141(6) 3_475 ? O2 Mn2 2.423(6) 3_475 ? O3 Mn1 2.111(6) 3_465 ? O3 Mn2 2.255(6) 3_475 ? O4 Mn2 2.137(7) 1_545 ? O4 Mn1 2.368(7) 3_465 ? O12 Mn1 2.214(6) 3_465 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mn1 O2 105.5(3) 3_565 3_575 ? O3 Mn1 O1 90.3(3) 3_565 . ? O2 Mn1 O1 96.5(3) 3_575 . ? O3 Mn1 O12 94.0(3) 3_565 3_565 ? O2 Mn1 O12 160.0(2) 3_575 3_565 ? O1 Mn1 O12 87.9(3) . 3_565 ? O3 Mn1 O10 93.0(3) 3_565 . ? O2 Mn1 O10 89.7(2) 3_575 . ? O1 Mn1 O10 172.0(4) . . ? O12 Mn1 O10 84.6(3) 3_565 . ? O3 Mn1 O4 157.3(2) 3_565 3_565 ? O2 Mn1 O4 97.0(3) 3_575 3_565 ? O1 Mn1 O4 84.7(3) . 3_565 ? O12 Mn1 O4 63.8(3) 3_565 3_565 ? O10 Mn1 O4 89.5(3) . 3_565 ? O3 Mn1 P1 125.59(18) 3_565 3_565 ? O2 Mn1 P1 128.89(17) 3_575 3_565 ? O1 Mn1 P1 84.1(2) . 3_565 ? O12 Mn1 P1 31.94(16) 3_565 3_565 ? O10 Mn1 P1 88.1(3) . 3_565 ? O4 Mn1 P1 31.94(16) 3_565 3_565 ? O12 Mn2 O5 93.4(2) . . ? O12 Mn2 O4 108.0(3) . 1_565 ? O5 Mn2 O4 91.9(2) . 1_565 ? O12 Mn2 O11 91.1(3) . . ? O5 Mn2 O11 173.9(3) . . ? O4 Mn2 O11 90.6(3) 1_565 . ? O12 Mn2 O3 153.5(2) . 3_575 ? O5 Mn2 O3 85.6(2) . 3_575 ? O4 Mn2 O3 98.5(3) 1_565 3_575 ? O11 Mn2 O3 88.5(3) . 3_575 ? O12 Mn2 O2 89.9(2) . 3_575 ? O5 Mn2 O2 84.2(2) . 3_575 ? O4 Mn2 O2 161.8(2) 1_565 3_575 ? O11 Mn2 O2 91.7(2) . 3_575 ? O3 Mn2 O2 63.6(2) 3_575 3_575 ? O12 Mn2 P2 121.87(18) . 3_575 ? O5 Mn2 P2 83.8(2) . 3_575 ? O4 Mn2 P2 130.04(18) 1_565 3_575 ? O11 Mn2 P2 90.3(3) . 3_575 ? O3 Mn2 P2 31.65(16) 3_575 3_575 ? O2 Mn2 P2 31.97(14) 3_575 3_575 ? O1 P1 O4 112.4(4) . . ? O1 P1 O12 114.1(4) . . ? O4 P1 O12 103.2(4) . . ? O1 P1 C2 109.9(5) . . ? O4 P1 C2 112.1(5) . . ? O12 P1 C2 104.8(5) . . ? O1 P1 Mn1 132.6(4) . 3_465 ? O4 P1 Mn1 54.5(3) . 3_465 ? O12 P1 Mn1 48.8(2) . 3_465 ? C2 P1 Mn1 117.1(4) . 3_465 ? O5 P2 O3 113.5(4) . . ? O5 P2 O2 113.3(3) . . ? O3 P2 O2 106.7(4) . . ? O5 P2 C1 110.9(5) . . ? O3 P2 C1 103.8(4) . . ? O2 P2 C1 108.1(4) . . ? O5 P2 Mn2 132.1(4) . 3_475 ? O3 P2 Mn2 50.2(2) . 3_475 ? O2 P2 Mn2 56.5(2) . 3_475 ? C1 P2 Mn2 116.7(3) . 3_475 ? C3 C1 P2 120.4(7) . . ? C9 C2 P1 116.9(8) . . ? C6 C3 C4 121.5(9) . . ? C6 C3 C1 119.1(8) . . ? C4 C3 C1 119.4(8) . . ? C3 C4 C7 118.2(9) . . ? C6 C5 C8 116.1(10) . . ? C3 C6 C5 123.3(9) . . ? C4 C7 C8 120.1(9) . . ? C5 C8 C15 121.7(10) . . ? C5 C8 C7 120.7(9) . . ? C15 C8 C7 117.5(9) . . ? C13 C9 C11 119.8(9) . . ? C13 C9 C2 121.4(9) . . ? C11 C9 C2 118.5(9) . . ? C12 C10 C13 116.9(9) . . ? C14 C11 C9 119.4(10) . . ? C14 C12 C10 123.1(9) . . ? C14 C12 C16 117.4(9) . . ? C10 C12 C16 119.4(9) . . ? C9 C13 C10 120.6(9) . . ? C12 C14 C11 119.8(10) . . ? O6 C15 O7 117.9(11) . . ? O6 C15 C8 125.7(11) . . ? O7 C15 C8 116.3(10) . . ? O9 C16 O8 123.1(10) . . ? O9 C16 C12 122.0(10) . . ? O8 C16 C12 114.5(10) . . ? P1 O1 Mn1 131.2(6) . . ? P2 O2 Mn1 123.7(4) . 3_475 ? P2 O2 Mn2 91.5(3) . 3_475 ? Mn1 O2 Mn2 116.3(3) 3_475 3_475 ? P2 O3 Mn1 128.0(4) . 3_465 ? P2 O3 Mn2 98.1(3) . 3_475 ? Mn1 O3 Mn2 121.8(3) 3_465 3_475 ? P1 O4 Mn2 124.0(4) . 1_545 ? P1 O4 Mn1 93.6(3) . 3_465 ? Mn2 O4 Mn1 118.2(3) 1_545 3_465 ? P2 O5 Mn2 131.4(5) . . ? P1 O12 Mn2 127.9(4) . . ? P1 O12 Mn1 99.2(3) . 3_465 ? Mn2 O12 Mn1 124.0(3) . 3_465 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 P2 C1 C3 50.9(8) . . . . ? O3 P2 C1 C3 173.1(7) . . . . ? O2 P2 C1 C3 -73.8(8) . . . . ? Mn2 P2 C1 C3 -134.8(7) 3_475 . . . ? O1 P1 C2 C9 53.4(9) . . . . ? O4 P1 C2 C9 -72.4(9) . . . . ? O12 P1 C2 C9 176.4(7) . . . . ? Mn1 P1 C2 C9 -132.6(7) 3_465 . . . ? P2 C1 C3 C6 85.1(10) . . . . ? P2 C1 C3 C4 -95.9(10) . . . . ? C6 C3 C4 C7 0.3(15) . . . . ? C1 C3 C4 C7 -178.7(9) . . . . ? C4 C3 C6 C5 -2.8(16) . . . . ? C1 C3 C6 C5 176.2(11) . . . . ? C8 C5 C6 C3 4.0(17) . . . . ? C3 C4 C7 C8 0.5(15) . . . . ? C6 C5 C8 C15 -179.8(10) . . . . ? C6 C5 C8 C7 -3.1(17) . . . . ? C4 C7 C8 C5 0.9(15) . . . . ? C4 C7 C8 C15 177.7(10) . . . . ? P1 C2 C9 C13 85.2(11) . . . . ? P1 C2 C9 C11 -100.8(11) . . . . ? C13 C9 C11 C14 -3.5(15) . . . . ? C2 C9 C11 C14 -177.6(10) . . . . ? C13 C10 C12 C14 5.7(15) . . . . ? C13 C10 C12 C16 -176.6(10) . . . . ? C11 C9 C13 C10 5.0(15) . . . . ? C2 C9 C13 C10 179.0(9) . . . . ? C12 C10 C13 C9 -6.0(15) . . . . ? C10 C12 C14 C11 -4.4(16) . . . . ? C16 C12 C14 C11 177.9(10) . . . . ? C9 C11 C14 C12 3.1(16) . . . . ? C5 C8 C15 O6 -177.9(12) . . . . ? C7 C8 C15 O6 5.3(17) . . . . ? C5 C8 C15 O7 2.8(16) . . . . ? C7 C8 C15 O7 -174.0(10) . . . . ? C14 C12 C16 O9 12.6(16) . . . . ? C10 C12 C16 O9 -165.2(11) . . . . ? C14 C12 C16 O8 -174.3(10) . . . . ? C10 C12 C16 O8 7.9(15) . . . . ? O4 P1 O1 Mn1 -68.6(6) . . . . ? O12 P1 O1 Mn1 48.5(6) . . . . ? C2 P1 O1 Mn1 165.8(5) . . . . ? Mn1 P1 O1 Mn1 -6.9(6) 3_465 . . . ? O3 Mn1 O1 P1 61.6(5) 3_565 . . . ? O2 Mn1 O1 P1 -44.1(5) 3_575 . . . ? O12 Mn1 O1 P1 155.6(5) 3_565 . . . ? O10 Mn1 O1 P1 175.7(11) . . . . ? O4 Mn1 O1 P1 -140.6(5) 3_565 . . . ? P1 Mn1 O1 P1 -172.6(4) 3_565 . . . ? O5 P2 O2 Mn1 2.8(6) . . . 3_475 ? O3 P2 O2 Mn1 -122.8(4) . . . 3_475 ? C1 P2 O2 Mn1 126.1(5) . . . 3_475 ? Mn2 P2 O2 Mn1 -123.3(4) 3_475 . . 3_475 ? O5 P2 O2 Mn2 126.1(4) . . . 3_475 ? O3 P2 O2 Mn2 0.5(4) . . . 3_475 ? C1 P2 O2 Mn2 -110.6(4) . . . 3_475 ? O5 P2 O3 Mn1 15.9(7) . . . 3_465 ? O2 P2 O3 Mn1 141.4(4) . . . 3_465 ? C1 P2 O3 Mn1 -104.6(5) . . . 3_465 ? Mn2 P2 O3 Mn1 141.9(6) 3_475 . . 3_465 ? O5 P2 O3 Mn2 -126.0(4) . . . 3_475 ? O2 P2 O3 Mn2 -0.6(5) . . . 3_475 ? C1 P2 O3 Mn2 113.5(4) . . . 3_475 ? O1 P1 O4 Mn2 -0.6(7) . . . 1_545 ? O12 P1 O4 Mn2 -123.9(4) . . . 1_545 ? C2 P1 O4 Mn2 123.8(5) . . . 1_545 ? Mn1 P1 O4 Mn2 -127.8(5) 3_465 . . 1_545 ? O1 P1 O4 Mn1 127.2(5) . . . 3_465 ? O12 P1 O4 Mn1 3.9(4) . . . 3_465 ? C2 P1 O4 Mn1 -108.4(4) . . . 3_465 ? O3 P2 O5 Mn2 50.4(5) . . . . ? O2 P2 O5 Mn2 -71.5(5) . . . . ? C1 P2 O5 Mn2 166.8(4) . . . . ? Mn2 P2 O5 Mn2 -6.4(5) 3_475 . . . ? O12 Mn2 O5 P2 -51.1(4) . . . . ? O4 Mn2 O5 P2 57.1(4) 1_565 . . . ? O11 Mn2 O5 P2 171.1(16) . . . . ? O3 Mn2 O5 P2 155.4(4) 3_575 . . . ? O2 Mn2 O5 P2 -140.7(4) 3_575 . . . ? P2 Mn2 O5 P2 -172.8(4) 3_575 . . . ? O1 P1 O12 Mn2 21.2(7) . . . . ? O4 P1 O12 Mn2 143.4(4) . . . . ? C2 P1 O12 Mn2 -99.1(5) . . . . ? Mn1 P1 O12 Mn2 147.6(6) 3_465 . . . ? O1 P1 O12 Mn1 -126.4(4) . . . 3_465 ? O4 P1 O12 Mn1 -4.2(5) . . . 3_465 ? C2 P1 O12 Mn1 113.3(4) . . . 3_465 ? O5 Mn2 O12 P1 -145.8(5) . . . . ? O4 Mn2 O12 P1 121.1(4) 1_565 . . . ? O11 Mn2 O12 P1 30.1(5) . . . . ? O3 Mn2 O12 P1 -58.9(9) 3_575 . . . ? O2 Mn2 O12 P1 -61.6(5) 3_575 . . . ? P2 Mn2 O12 P1 -61.0(5) 3_575 . . . ? O5 Mn2 O12 Mn1 -5.4(4) . . . 3_465 ? O4 Mn2 O12 Mn1 -98.5(4) 1_565 . . 3_465 ? O11 Mn2 O12 Mn1 170.5(4) . . . 3_465 ? O3 Mn2 O12 Mn1 81.5(6) 3_575 . . 3_465 ? O2 Mn2 O12 Mn1 78.8(3) 3_575 . . 3_465 ? P2 Mn2 O12 Mn1 79.4(4) 3_575 . . 3_465 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.143 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.193