 
data_exp_12906 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C10 H13 Mn O8' 
_chemical_formula_sum 
 'C10 H13 Mn N0 O8' 
_chemical_formula_weight          316.14 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Mn'  'Mn'  -0.5299   2.8052 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            triclinic 
_symmetry_space_group_name_H-M    P-1
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    8.1304(7) 
_cell_length_b                    8.2667(10) 
_cell_length_c                    10.0751(7) 
_cell_angle_alpha                 80.531(8) 
_cell_angle_beta                  70.026(7) 
_cell_angle_gamma                 83.552(8) 
_cell_volume                      626.60(10) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     1905
_cell_measurement_theta_min       4.4200
_cell_measurement_theta_max       71.1190 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             pink 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.676 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              324 
_exptl_absorpt_coefficient_mu     8.918 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.29792
_exptl_absorpt_correction_T_max   1.00000 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      1.54184 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'four-circle diffractometer' 
_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             3815 
_diffrn_reflns_av_R_equivalents   0.0584 
_diffrn_reflns_av_sigmaI/netI     0.0660 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          4.71 
_diffrn_reflns_theta_max          71.21 
_reflns_number_total              2346 
_reflns_number_gt                 2000 
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1689P)²+0.0000P] where P=(Fo²+2Fc²)/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          2346 
_refine_ls_number_parameters      172 
_refine_ls_number_restraints      401 
_refine_ls_R_factor_all           0.0892 
_refine_ls_R_factor_gt            0.0807 
_refine_ls_wR_factor_ref          0.2389 
_refine_ls_wR_factor_gt           0.2211 
_refine_ls_goodness_of_fit_ref    1.089 
_refine_ls_restrained_S_all       1.109 
_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 
O3 O 0.0470(6) 0.6047(6) 0.8407(5) 0.0572(11) Uani 1 1 d U . . 
C10 C 0.2029(7) 0.6412(7) 0.8070(5) 0.0332(10) Uani 1 1 d U . . 
O4 O 0.2719(6) 0.6550(6) 0.8982(4) 0.0501(10) Uani 1 1 d U . . 
Mn1 Mn 0.15303(9) 0.55241(10) 0.11252(7) 0.0331(4) Uani 1 1 d U . . 
O5 O 0.1589(5) 0.5379(5) 0.3301(4) 0.0404(9) Uani 1 1 d U . . 
O6 O 0.3621(5) 0.6801(5) 0.1662(4) 0.0412(9) Uani 1 1 d U . . 
O7 O 0.7320(4) 0.8384(5) 0.4245(4) 0.0332(8) Uani 1 1 d U . . 
C2 C 0.3529(6) 0.6654(6) 0.4061(5) 0.0246(9) Uani 1 1 d U . . 
C4 C 0.5718(6) 0.7733(6) 0.4730(5) 0.0247(9) Uani 1 1 d U . . 
C1 C 0.2879(6) 0.6238(6) 0.2940(5) 0.0284(9) Uani 1 1 d U . . 
C3 C 0.5104(6) 0.7349(6) 0.3689(5) 0.0270(9) Uani 1 1 d U . . 
H3 H 0.5774 0.7568 0.2732 0.032 Uiso 1 1 calc R . . 
O1 O -0.0319(6) 0.7731(7) 0.1534(5) 0.0618(13) Uani 1 1 d U . . 
H1B H 0.0336 0.8696 0.1291 0.093 Uiso 1 1 d R . . 
H1C H -0.1017 0.7629 0.2525 0.093 Uiso 1 1 d R . . 
C5 C 0.4696(6) 0.7441(6) 0.6146(5) 0.0265(9) Uani 1 1 d U . . 
H5 H 0.5083 0.7710 0.6846 0.032 Uiso 1 1 calc R . . 
C7 C 0.2499(6) 0.6332(6) 0.5489(5) 0.0268(9) Uani 1 1 d U . . 
H7 H 0.1435 0.5848 0.5748 0.032 Uiso 1 1 calc R . . 
C8 C 0.7965(6) 0.8862(7) 0.5279(5) 0.0308(10) Uani 1 1 d U . . 
H8A H 0.8166 0.7904 0.5916 0.037 Uiso 1 1 calc R . . 
H8B H 0.7116 0.9617 0.5842 0.037 Uiso 1 1 calc R . . 
C6 C 0.3105(6) 0.6755(6) 0.6526(5) 0.0256(9) Uani 1 1 d U . . 
C9 C 0.9656(6) 0.9679(6) 0.4483(5) 0.0282(10) Uani 1 1 d U . . 
H9A H 0.9462 1.0583 0.3795 0.034 Uiso 1 1 calc R . . 
H9B H 1.0520 0.8896 0.3967 0.034 Uiso 1 1 calc R . . 
O2 O 0.3437(8) 0.3388(7) 0.0708(7) 0.0775(17) Uani 1 1 d U . . 
H2A H 0.3245 0.2829 0.0016 0.116 Uiso 1 1 d R . . 
H2C H 0.4606 0.3759 0.0349 0.116 Uiso 1 1 d R . . 
O8 O 0.7853(16) 0.9540(13) 0.9724(12) 0.174(5) Uani 1 1 d D . . 
H8E H 0.8743 0.8915 0.9358 0.209 Uiso 1 1 d RD . . 
H8C H 0.7904 0.9839 1.0476 0.209 Uiso 1 1 d RD . . 
 
 
_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 
O3 C10 1.253(7) . ? 
O3 Mn1 2.075(4) 2_566 ? 
C10 O4 1.255(6) . ? 
C10 C6 1.499(6) . ? 
O4 Mn1 2.114(4) 1_556 ? 
Mn1 O3 2.075(4) 2_566 ? 
Mn1 O4 2.114(4) 1_554 ? 
Mn1 O5 2.192(4) . ? 
Mn1 O2 2.210(6) . ? 
Mn1 O1 2.229(5) . ? 
Mn1 O6 2.348(4) . ? 
Mn1 C1 2.600(5) . ? 
O5 C1 1.248(6) . ? 
O6 C1 1.255(6) . ? 
O7 C4 1.364(6) . ? 
O7 C8 1.440(5) . ? 
C2 C3 1.370(6) . ? 
C2 C7 1.394(6) . ? 
C2 C1 1.501(6) . ? 
C4 C5 1.381(6) . ? 
C4 C3 1.397(6) . ? 
C5 C6 1.377(6) . ? 
C7 C6 1.402(6) . ? 
C8 C9 1.505(6) . ? 
C9 C9 1.526(8) 2_776 ? 
 
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 
C10 O3 Mn1 155.4(5) . 2_566 ? 
O3 C10 O4 122.3(5) . . ? 
O3 C10 C6 119.5(4) . . ? 
O4 C10 C6 118.1(4) . . ? 
C10 O4 Mn1 119.4(3) . 1_556 ? 
O3 Mn1 O4 118.66(17) 2_566 1_554 ? 
O3 Mn1 O5 97.09(15) 2_566 . ? 
O4 Mn1 O5 144.22(15) 1_554 . ? 
O3 Mn1 O2 88.7(2) 2_566 . ? 
O4 Mn1 O2 88.1(2) 1_554 . ? 
O5 Mn1 O2 91.6(2) . . ? 
O3 Mn1 O1 93.3(2) 2_566 . ? 
O4 Mn1 O1 91.06(19) 1_554 . ? 
O5 Mn1 O1 87.97(18) . . ? 
O2 Mn1 O1 178.07(19) . . ? 
O3 Mn1 O6 154.08(17) 2_566 . ? 
O4 Mn1 O6 86.87(15) 1_554 . ? 
O5 Mn1 O6 57.39(13) . . ? 
O2 Mn1 O6 87.7(2) . . ? 
O1 Mn1 O6 90.45(18) . . ? 
O3 Mn1 C1 125.58(17) 2_566 . ? 
O4 Mn1 C1 115.64(16) 1_554 . ? 
O5 Mn1 C1 28.59(14) . . ? 
O2 Mn1 C1 89.9(2) . . ? 
O1 Mn1 C1 88.90(18) . . ? 
O6 Mn1 C1 28.80(15) . . ? 
C1 O5 Mn1 94.2(3) . . ? 
C1 O6 Mn1 86.8(3) . . ? 
C4 O7 C8 117.7(4) . . ? 
C3 C2 C7 120.5(4) . . ? 
C3 C2 C1 120.6(4) . . ? 
C7 C2 C1 118.9(4) . . ? 
O7 C4 C5 124.8(4) . . ? 
O7 C4 C3 116.0(4) . . ? 
C5 C4 C3 119.2(4) . . ? 
O5 C1 O6 121.6(4) . . ? 
O5 C1 C2 119.5(4) . . ? 
O6 C1 C2 118.9(4) . . ? 
O5 C1 Mn1 57.2(2) . . ? 
O6 C1 Mn1 64.4(3) . . ? 
C2 C1 Mn1 176.0(3) . . ? 
C2 C3 C4 120.8(4) . . ? 
C6 C5 C4 120.2(4) . . ? 
C2 C7 C6 118.4(4) . . ? 
O7 C8 C9 107.8(4) . . ? 
C5 C6 C7 120.9(4) . . ? 
C5 C6 C10 119.6(4) . . ? 
C7 C6 C10 119.5(4) . . ? 
C8 C9 C9 110.3(5) . 2_776 ? 
 
_diffrn_measured_fraction_theta_max    0.970 
_diffrn_reflns_theta_full              71.21 
_diffrn_measured_fraction_theta_full   0.970 
_refine_diff_density_max    1.529 
_refine_diff_density_min   -1.091 
_refine_diff_density_rms    0.200 
