data_sol1m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H20 Mn N2 O14 P4' _chemical_formula_weight 499.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? 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 7.3668(11) _cell_length_b 8.1540(12) _cell_length_c 14.090(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.935(2) _cell_angle_gamma 90.00 _cell_volume 821.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 510 _exptl_absorpt_coefficient_mu 1.269 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 9094 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 28.20 _reflns_number_total 1947 _reflns_number_gt 1897 _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^)+(0.0000P)^2^+3.0229P] 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 1947 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0870 _refine_ls_goodness_of_fit_ref 1.311 _refine_ls_restrained_S_all 1.311 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 1.0000 1.0000 0.01215(16) Uani 1 2 d S . . P1 P 0.18439(10) 0.77382(9) 0.84370(5) 0.01023(17) Uani 1 1 d . . . P2 P 0.07290(10) 0.68356(9) 1.15777(5) 0.01020(17) Uani 1 1 d . . . O1 O 0.2872(3) 0.6125(3) 0.85485(15) 0.0125(4) Uani 1 1 d . . . O5 O -0.1127(3) 0.6217(3) 1.08865(17) 0.0148(5) Uani 1 1 d . . . O3 O 0.0680(3) 0.8047(3) 0.91512(15) 0.0137(4) Uani 1 1 d . . . O4 O 0.0851(3) 0.6430(3) 1.26334(15) 0.0154(5) Uani 1 1 d . . . N1 N -0.0682(4) 0.9401(3) 0.70274(19) 0.0109(5) Uani 1 1 d . . . O2 O 0.3191(3) 0.9217(3) 0.84456(16) 0.0138(4) Uani 1 1 d . . . O6 O 0.0961(3) 0.8616(3) 1.13611(15) 0.0122(4) Uani 1 1 d . . . C2 C 0.0278(4) 0.7770(4) 0.7225(2) 0.0118(6) Uani 1 1 d . . . O1W O 0.2824(4) 1.1038(4) 1.0305(2) 0.0250(6) Uani 1 1 d . . . C1 C 0.2547(4) 0.5625(4) 1.1232(2) 0.0122(6) Uani 1 1 d . . . H1WB H 0.341(8) 1.064(8) 1.004(5) 0.06(2) Uiso 1 1 d . . . H2C H 0.402(5) 0.897(5) 0.813(3) 0.016(9) Uiso 1 1 d . . . H2B H -0.060(5) 0.693(4) 0.719(2) 0.005(8) Uiso 1 1 d . . . H1B H 0.282(5) 0.607(5) 1.065(3) 0.018(10) Uiso 1 1 d . . . H1D H -0.094(5) 0.977(5) 0.758(3) 0.018(10) Uiso 1 1 d . . . H1A H 0.214(6) 0.451(5) 1.112(3) 0.023(10) Uiso 1 1 d . . . H2A H 0.098(5) 0.762(5) 0.674(3) 0.014(9) Uiso 1 1 d . . . H1C H 0.009(6) 1.008(5) 0.690(3) 0.021(10) Uiso 1 1 d . . . H5A H -0.156(7) 0.556(6) 1.107(3) 0.036(14) Uiso 1 1 d . . . H1WA H 0.323(9) 1.128(8) 1.089(5) 0.07(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0149(3) 0.0119(3) 0.0095(3) -0.0001(2) 0.0027(2) 0.0038(2) P1 0.0107(3) 0.0094(3) 0.0110(3) -0.0007(3) 0.0034(3) 0.0002(3) P2 0.0095(3) 0.0104(4) 0.0107(3) 0.0006(3) 0.0024(3) 0.0011(3) O1 0.0123(10) 0.0098(10) 0.0163(10) -0.0006(8) 0.0052(8) 0.0007(8) O5 0.0142(11) 0.0136(11) 0.0154(11) 0.0033(9) 0.0010(9) -0.0025(9) O3 0.0163(11) 0.0119(10) 0.0147(10) -0.0002(8) 0.0074(8) 0.0010(8) O4 0.0141(10) 0.0205(11) 0.0130(10) 0.0039(9) 0.0059(8) 0.0035(9) N1 0.0098(11) 0.0114(12) 0.0124(12) -0.0001(9) 0.0043(10) 0.0008(9) O2 0.0143(10) 0.0131(10) 0.0149(10) 0.0003(8) 0.0054(9) -0.0009(8) O6 0.0137(10) 0.0105(10) 0.0121(10) -0.0006(8) 0.0027(8) 0.0000(8) C2 0.0115(13) 0.0112(14) 0.0121(14) -0.0003(11) 0.0018(11) 0.0005(11) O1W 0.0217(13) 0.0317(15) 0.0193(13) 0.0018(11) 0.0002(11) -0.0089(12) C1 0.0131(14) 0.0111(14) 0.0122(13) -0.0021(11) 0.0023(11) -0.0002(11) _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 2.123(2) 3_577 ? Mn1 O3 2.123(2) . ? Mn1 O6 2.191(2) . ? Mn1 O6 2.191(2) 3_577 ? Mn1 O1W 2.191(3) 3_577 ? Mn1 O1W 2.191(3) . ? P1 O3 1.492(2) . ? P1 O1 1.507(2) . ? P1 O2 1.560(2) . ? P1 C2 1.816(3) . ? P2 O6 1.502(2) . ? P2 O4 1.505(2) . ? P2 O5 1.559(2) . ? P2 C1 1.822(3) . ? N1 C2 1.500(4) . ? N1 C1 1.501(4) 4_575 ? C1 N1 1.501(4) 4_676 ? 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 O3 180.000(1) 3_577 . ? O3 Mn1 O6 87.92(8) 3_577 . ? O3 Mn1 O6 92.08(8) . . ? O3 Mn1 O6 92.08(8) 3_577 3_577 ? O3 Mn1 O6 87.92(8) . 3_577 ? O6 Mn1 O6 180.000(1) . 3_577 ? O3 Mn1 O1W 93.35(11) 3_577 3_577 ? O3 Mn1 O1W 86.65(11) . 3_577 ? O6 Mn1 O1W 93.67(9) . 3_577 ? O6 Mn1 O1W 86.33(9) 3_577 3_577 ? O3 Mn1 O1W 86.65(11) 3_577 . ? O3 Mn1 O1W 93.35(11) . . ? O6 Mn1 O1W 86.33(9) . . ? O6 Mn1 O1W 93.67(9) 3_577 . ? O1W Mn1 O1W 180.00(16) 3_577 . ? O3 P1 O1 115.64(13) . . ? O3 P1 O2 109.42(13) . . ? O1 P1 O2 111.77(12) . . ? O3 P1 C2 107.07(14) . . ? O1 P1 C2 107.46(13) . . ? O2 P1 C2 104.78(13) . . ? O6 P2 O4 115.52(13) . . ? O6 P2 O5 108.13(13) . . ? O4 P2 O5 112.40(13) . . ? O6 P2 C1 110.02(14) . . ? O4 P2 C1 105.78(13) . . ? O5 P2 C1 104.39(14) . . ? P1 O3 Mn1 139.30(13) . . ? C2 N1 C1 114.3(2) . 4_575 ? P2 O6 Mn1 130.35(12) . . ? N1 C2 P1 110.6(2) . . ? N1 C1 P2 111.8(2) 4_676 . ? 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 O1 P1 O3 Mn1 139.78(18) . . . . ? O2 P1 O3 Mn1 12.5(2) . . . . ? C2 P1 O3 Mn1 -100.5(2) . . . . ? O3 Mn1 O3 P1 63(100) 3_577 . . . ? O6 Mn1 O3 P1 -123.4(2) . . . . ? O6 Mn1 O3 P1 56.6(2) 3_577 . . . ? O1W Mn1 O3 P1 143.0(2) 3_577 . . . ? O1W Mn1 O3 P1 -37.0(2) . . . . ? O4 P2 O6 Mn1 -156.20(14) . . . . ? O5 P2 O6 Mn1 -29.3(2) . . . . ? C1 P2 O6 Mn1 84.15(18) . . . . ? O3 Mn1 O6 P2 139.66(17) 3_577 . . . ? O3 Mn1 O6 P2 -40.34(17) . . . . ? O6 Mn1 O6 P2 2(100) 3_577 . . . ? O1W Mn1 O6 P2 46.43(18) 3_577 . . . ? O1W Mn1 O6 P2 -133.57(18) . . . . ? C1 N1 C2 P1 -159.2(2) 4_575 . . . ? O3 P1 C2 N1 59.9(2) . . . . ? O1 P1 C2 N1 -175.29(19) . . . . ? O2 P1 C2 N1 -56.3(2) . . . . ? O6 P2 C1 N1 84.6(2) . . . 4_676 ? O4 P2 C1 N1 -40.8(2) . . . 4_676 ? O5 P2 C1 N1 -159.6(2) . . . 4_676 ? 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 O1W H1WB O2 0.71(6) 2.50(6) 3.079(4) 140(6) . O2 H2C O4 0.86(4) 1.69(4) 2.551(3) 173(4) 4_675 N1 H1D O6 0.89(4) 1.99(4) 2.835(3) 156(4) 3_577 O5 H5A O1 0.70(5) 1.84(5) 2.535(3) 175(6) 3_567 O1W H1WA O4 0.83(7) 2.03(7) 2.851(4) 169(6) 2_557 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.548 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.097