data_2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C17 H16 Mn N5 O8 S' 
_chemical_formula_weight          505.35 
 
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' 
 'Mn'  'Mn'   0.3368   0.7283 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P21/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                    13.9356(18) 
_cell_length_b                    12.7072(16) 
_cell_length_c                    13.0672(16) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  116.187(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2076.5(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     6471 
_cell_measurement_theta_min       2.28
_cell_measurement_theta_max       29.96
 
_exptl_crystal_description        block 
_exptl_crystal_colour             brown
_exptl_crystal_size_max           0.27 
_exptl_crystal_size_mid           0.26 
_exptl_crystal_size_min           0.22 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.617 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1032 
_exptl_absorpt_coefficient_mu     0.793 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8144 
_exptl_absorpt_correction_T_max   0.8449 
_exptl_absorpt_process_details    SADABS
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   'Bruker SMART CCD area-detector'
_diffrn_measurement_method        '\w scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          0 
_diffrn_standards_interval_count  . 
_diffrn_standards_interval_time   . 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11814 
_diffrn_reflns_av_R_equivalents   0.0170 
_diffrn_reflns_av_sigmaI/netI     0.0199 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.28 
_diffrn_reflns_theta_max          27.00 
_reflns_number_total              4516 
_reflns_number_gt                 3623 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        SMART 
_computing_cell_refinement        SAINT
_computing_data_reduction         SAINT 
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material   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^)+(0.0696P)^2^+1.2371P] 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          4516 
_refine_ls_number_parameters      301 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.0538 
_refine_ls_R_factor_gt            0.0411 
_refine_ls_wR_factor_ref          0.1294 
_refine_ls_wR_factor_gt           0.1148 
_refine_ls_goodness_of_fit_ref    1.050 
_refine_ls_restrained_S_all       1.050 
_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 0.10247(3) 0.94225(3) 0.38933(3) 0.04064(14) Uani 1 1 d . . . 
N1 N 0.24357(16) 0.87326(15) 0.47186(19) 0.0450(5) Uani 1 1 d . . . 
N2 N 0.05908(16) 0.80137(16) 0.3194(2) 0.0469(5) Uani 1 1 d . . . 
N3 N 0.5692(2) 1.2203(2) 0.6950(2) 0.0655(7) Uani 1 1 d . . . 
N4 N -0.4227(2) 0.7708(3) 0.1150(2) 0.0693(8) Uani 1 1 d . . . 
N5 N 0.1468(2) 0.9957(2) 0.2554(2) 0.0627(6) Uani 1 1 d . . . 
O1 O 0.15384(12) 1.06689(13) 0.47398(16) 0.0456(4) Uani 1 1 d . . . 
O2 O -0.04120(12) 0.99277(13) 0.31381(15) 0.0441(4) Uani 1 1 d . . . 
O3 O 0.06526(16) 0.87051(16) 0.52919(19) 0.0565(5) Uani 1 1 d D . . 
O4 O 0.5816(2) 1.3105(2) 0.7287(3) 0.0954(9) Uani 1 1 d . . . 
O5 O 0.64232(18) 1.1650(2) 0.7014(3) 0.1001(9) Uani 1 1 d . . . 
O6 O -0.50523(19) 0.8215(3) 0.0715(3) 0.1092(11) Uani 1 1 d . . . 
O7 O -0.4200(2) 0.6752(2) 0.1189(2) 0.0869(8) Uani 1 1 d . . . 
O8 O -0.0016(3) 0.6700(2) 0.5185(4) 0.1297(13) Uani 1 1 d D . . 
S1 S 0.20637(12) 1.01094(9) 0.07945(12) 0.1041(4) Uani 1 1 d . . . 
C1 C 0.34310(18) 1.0309(2) 0.5555(2) 0.0410(5) Uani 1 1 d . . . 
C2 C 0.25344(17) 1.09843(19) 0.5278(2) 0.0385(5) Uani 1 1 d . . . 
C3 C 0.2727(2) 1.2044(2) 0.5616(2) 0.0450(5) Uani 1 1 d . . . 
H3 H 0.2149 1.2489 0.5466 0.054 Uiso 1 1 calc R . . 
C4 C 0.3748(2) 1.2439(2) 0.6163(2) 0.0495(6) Uani 1 1 d . . . 
H4 H 0.3861 1.3146 0.6366 0.059 Uiso 1 1 calc R . . 
C5 C 0.46054(19) 1.1770(2) 0.6409(2) 0.0498(6) Uani 1 1 d . . . 
C6 C 0.44675(19) 1.0723(2) 0.6127(2) 0.0484(6) Uani 1 1 d . . . 
H6 H 0.5059 1.0289 0.6315 0.058 Uiso 1 1 calc R . . 
C7 C 0.33170(18) 0.9202(2) 0.5303(2) 0.0451(6) Uani 1 1 d . . . 
H7 H 0.3936 0.8796 0.5590 0.054 Uiso 1 1 calc R . . 
C8 C 0.2374(2) 0.7575(2) 0.4579(3) 0.0615(8) Uani 1 1 d . . . 
H8A H 0.2197 0.7253 0.5148 0.074 Uiso 1 1 calc R . . 
H8B H 0.3056 0.7298 0.4672 0.074 Uiso 1 1 calc R . . 
C9 C 0.1515(2) 0.7335(2) 0.3396(3) 0.0624(8) Uani 1 1 d . . . 
H9A H 0.1776 0.7477 0.2833 0.075 Uiso 1 1 calc R . . 
H9B H 0.1311 0.6600 0.3339 0.075 Uiso 1 1 calc R . . 
C10 C -0.0365(2) 0.7666(2) 0.2694(2) 0.0493(6) Uani 1 1 d . . . 
H10 H -0.0458 0.6962 0.2474 0.059 Uiso 1 1 calc R . . 
C11 C -0.13123(19) 0.8279(2) 0.2445(2) 0.0436(5) Uani 1 1 d . . . 
C12 C -0.13021(18) 0.93769(18) 0.2656(2) 0.0393(5) Uani 1 1 d . . . 
C13 C -0.22840(19) 0.9901(2) 0.2334(2) 0.0470(6) Uani 1 1 d . . . 
H13 H -0.2287 1.0618 0.2478 0.056 Uiso 1 1 calc R . . 
C14 C -0.3238(2) 0.9370(2) 0.1811(2) 0.0527(6) Uani 1 1 d . . . 
H14 H -0.3883 0.9726 0.1574 0.063 Uiso 1 1 calc R . . 
C15 C -0.3224(2) 0.8297(2) 0.1642(2) 0.0518(6) Uani 1 1 d . . . 
C16 C -0.2296(2) 0.7749(2) 0.1955(2) 0.0503(6) Uani 1 1 d . . . 
H16 H -0.2315 0.7025 0.1845 0.060 Uiso 1 1 calc R . . 
C17 C 0.1731(3) 1.0021(2) 0.1849(3) 0.0620(7) Uani 1 1 d . . . 
H8C H -0.0494(19) 0.621(2) 0.499(3) 0.080 Uiso 1 1 d D . . 
H8D H 0.0552(15) 0.633(2) 0.538(3) 0.080 Uiso 1 1 d D . . 
H3B H 0.047(3) 0.906(2) 0.572(3) 0.080 Uiso 1 1 d D . . 
H3A H 0.032(3) 0.8128(15) 0.515(3) 0.080 Uiso 1 1 d 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 0.02607(19) 0.0334(2) 0.0566(2) -0.00558(15) 0.01293(16) -0.00002(12) 
N1 0.0326(10) 0.0371(10) 0.0626(13) 0.0007(9) 0.0184(9) 0.0060(8) 
N2 0.0385(10) 0.0409(11) 0.0626(13) -0.0102(9) 0.0234(10) -0.0019(8) 
N3 0.0412(13) 0.0824(19) 0.0688(16) -0.0128(14) 0.0206(11) -0.0183(13) 
N4 0.0450(14) 0.098(2) 0.0658(16) -0.0225(15) 0.0258(12) -0.0303(14) 
N5 0.0574(14) 0.0651(16) 0.0729(16) 0.0045(13) 0.0353(13) -0.0001(12) 
O1 0.0265(8) 0.0400(9) 0.0631(10) -0.0097(7) 0.0133(7) 0.0006(6) 
O2 0.0261(7) 0.0376(8) 0.0598(10) -0.0042(7) 0.0109(7) -0.0033(6) 
O3 0.0547(11) 0.0508(11) 0.0704(13) -0.0085(9) 0.0336(10) -0.0015(9) 
O4 0.0649(15) 0.096(2) 0.118(2) -0.0462(17) 0.0336(15) -0.0403(14) 
O5 0.0369(11) 0.104(2) 0.148(3) -0.0196(19) 0.0311(14) -0.0132(13) 
O6 0.0358(12) 0.131(3) 0.135(3) -0.026(2) 0.0138(14) -0.0256(15) 
O7 0.0715(16) 0.0940(19) 0.1038(19) -0.0399(16) 0.0465(14) -0.0498(14) 
O8 0.121(3) 0.0574(17) 0.173(4) 0.014(2) 0.031(3) -0.0019(17) 
S1 0.1558(12) 0.0709(6) 0.1375(10) 0.0058(6) 0.1121(10) 0.0045(7) 
C1 0.0296(11) 0.0466(12) 0.0459(12) 0.0004(10) 0.0156(9) 0.0009(9) 
C2 0.0306(10) 0.0427(12) 0.0419(11) -0.0020(10) 0.0158(9) -0.0010(9) 
C3 0.0387(12) 0.0470(13) 0.0486(13) -0.0061(11) 0.0187(10) -0.0011(10) 
C4 0.0494(14) 0.0494(14) 0.0506(14) -0.0114(11) 0.0228(11) -0.0103(11) 
C5 0.0345(12) 0.0649(16) 0.0482(13) -0.0087(12) 0.0167(10) -0.0121(11) 
C6 0.0295(11) 0.0620(16) 0.0527(14) -0.0010(12) 0.0172(10) 0.0001(10) 
C7 0.0279(11) 0.0494(13) 0.0563(14) 0.0040(11) 0.0170(10) 0.0085(9) 
C8 0.0399(13) 0.0377(13) 0.101(2) 0.0002(14) 0.0263(14) 0.0079(11) 
C9 0.0488(15) 0.0425(14) 0.100(2) -0.0198(15) 0.0363(15) 0.0006(11) 
C10 0.0478(14) 0.0392(12) 0.0625(16) -0.0132(11) 0.0257(12) -0.0083(10) 
C11 0.0362(11) 0.0493(13) 0.0445(12) -0.0092(10) 0.0171(10) -0.0100(10) 
C12 0.0307(11) 0.0424(12) 0.0421(12) -0.0009(9) 0.0136(9) -0.0054(9) 
C13 0.0324(11) 0.0509(14) 0.0533(14) 0.0041(11) 0.0149(10) -0.0035(10) 
C14 0.0289(12) 0.0716(18) 0.0536(14) 0.0040(13) 0.0145(10) -0.0035(11) 
C15 0.0372(13) 0.0710(18) 0.0451(13) -0.0118(12) 0.0161(10) -0.0207(12) 
C16 0.0464(14) 0.0555(15) 0.0506(14) -0.0151(12) 0.0229(11) -0.0182(11) 
C17 0.0640(18) 0.0410(15) 0.085(2) -0.0025(14) 0.0362(17) -0.0040(13) 
 
_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 O1 1.8830(16) . ? 
Mn1 O2 1.9107(16) . ? 
Mn1 N2 1.979(2) . ? 
Mn1 N1 1.981(2) . ? 
Mn1 N5 2.205(3) . ? 
Mn1 O3 2.297(2) . ? 
N1 C7 1.272(3) . ? 
N1 C8 1.480(3) . ? 
N2 C10 1.277(3) . ? 
N2 C9 1.474(3) . ? 
N3 O5 1.210(4) . ? 
N3 O4 1.212(4) . ? 
N3 C5 1.466(3) . ? 
N4 O7 1.215(4) . ? 
N4 O6 1.219(4) . ? 
N4 C15 1.460(3) . ? 
N5 C17 1.135(4) . ? 
O1 C2 1.312(3) . ? 
O2 C12 1.317(3) . ? 
O3 H3B 0.846(10) . ? 
O3 H3A 0.844(10) . ? 
O8 H8C 0.866(10) . ? 
O8 H8D 0.860(10) . ? 
S1 C17 1.640(4) . ? 
C1 C6 1.403(3) . ? 
C1 C2 1.425(3) . ? 
C1 C7 1.438(4) . ? 
C2 C3 1.406(3) . ? 
C3 C4 1.375(4) . ? 
C3 H3 0.9300 . ? 
C4 C5 1.384(4) . ? 
C4 H4 0.9300 . ? 
C5 C6 1.371(4) . ? 
C6 H6 0.9300 . ? 
C7 H7 0.9300 . ? 
C8 C9 1.511(5) . ? 
C8 H8A 0.9700 . ? 
C8 H8B 0.9700 . ? 
C9 H9A 0.9700 . ? 
C9 H9B 0.9700 . ? 
C10 C11 1.440(4) . ? 
C10 H10 0.9300 . ? 
C11 C16 1.403(3) . ? 
C11 C12 1.421(3) . ? 
C12 C13 1.409(3) . ? 
C13 C14 1.374(3) . ? 
C13 H13 0.9300 . ? 
C14 C15 1.382(4) . ? 
C14 H14 0.9300 . ? 
C15 C16 1.363(4) . ? 
C16 H16 0.9300 . ? 
 
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 Mn1 O2 93.49(7) . . ? 
O1 Mn1 N2 172.49(9) . . ? 
O2 Mn1 N2 91.63(8) . . ? 
O1 Mn1 N1 91.36(8) . . ? 
O2 Mn1 N1 172.62(8) . . ? 
N2 Mn1 N1 83.04(9) . . ? 
O1 Mn1 N5 92.31(9) . . ? 
O2 Mn1 N5 94.78(9) . . ? 
N2 Mn1 N5 92.74(10) . . ? 
N1 Mn1 N5 90.58(10) . . ? 
O1 Mn1 O3 91.55(8) . . ? 
O2 Mn1 O3 89.49(8) . . ? 
N2 Mn1 O3 83.00(8) . . ? 
N1 Mn1 O3 84.81(8) . . ? 
N5 Mn1 O3 174.06(9) . . ? 
C7 N1 C8 121.9(2) . . ? 
C7 N1 Mn1 125.63(17) . . ? 
C8 N1 Mn1 112.51(16) . . ? 
C10 N2 C9 121.4(2) . . ? 
C10 N2 Mn1 125.93(18) . . ? 
C9 N2 Mn1 112.44(16) . . ? 
O5 N3 O4 122.9(3) . . ? 
O5 N3 C5 118.3(3) . . ? 
O4 N3 C5 118.8(3) . . ? 
O7 N4 O6 123.6(3) . . ? 
O7 N4 C15 119.2(3) . . ? 
O6 N4 C15 117.2(3) . . ? 
C17 N5 Mn1 166.1(3) . . ? 
C2 O1 Mn1 127.59(15) . . ? 
C12 O2 Mn1 128.27(15) . . ? 
Mn1 O3 H3B 124(2) . . ? 
Mn1 O3 H3A 118(2) . . ? 
H3B O3 H3A 108(2) . . ? 
H8C O8 H8D 100(2) . . ? 
C6 C1 C2 119.4(2) . . ? 
C6 C1 C7 118.2(2) . . ? 
C2 C1 C7 122.4(2) . . ? 
O1 C2 C3 118.1(2) . . ? 
O1 C2 C1 123.6(2) . . ? 
C3 C2 C1 118.2(2) . . ? 
C4 C3 C2 121.5(2) . . ? 
C4 C3 H3 119.2 . . ? 
C2 C3 H3 119.2 . . ? 
C3 C4 C5 119.1(2) . . ? 
C3 C4 H4 120.4 . . ? 
C5 C4 H4 120.4 . . ? 
C6 C5 C4 122.0(2) . . ? 
C6 C5 N3 119.1(2) . . ? 
C4 C5 N3 118.9(3) . . ? 
C5 C6 C1 119.7(2) . . ? 
C5 C6 H6 120.1 . . ? 
C1 C6 H6 120.1 . . ? 
N1 C7 C1 125.1(2) . . ? 
N1 C7 H7 117.4 . . ? 
C1 C7 H7 117.4 . . ? 
N1 C8 C9 107.7(2) . . ? 
N1 C8 H8A 110.2 . . ? 
C9 C8 H8A 110.2 . . ? 
N1 C8 H8B 110.2 . . ? 
C9 C8 H8B 110.2 . . ? 
H8A C8 H8B 108.5 . . ? 
N2 C9 C8 107.5(2) . . ? 
N2 C9 H9A 110.2 . . ? 
C8 C9 H9A 110.2 . . ? 
N2 C9 H9B 110.2 . . ? 
C8 C9 H9B 110.2 . . ? 
H9A C9 H9B 108.5 . . ? 
N2 C10 C11 125.0(2) . . ? 
N2 C10 H10 117.5 . . ? 
C11 C10 H10 117.5 . . ? 
C16 C11 C12 118.9(2) . . ? 
C16 C11 C10 117.2(2) . . ? 
C12 C11 C10 123.9(2) . . ? 
O2 C12 C13 118.5(2) . . ? 
O2 C12 C11 122.8(2) . . ? 
C13 C12 C11 118.8(2) . . ? 
C14 C13 C12 121.0(3) . . ? 
C14 C13 H13 119.5 . . ? 
C12 C13 H13 119.5 . . ? 
C13 C14 C15 119.1(3) . . ? 
C13 C14 H14 120.5 . . ? 
C15 C14 H14 120.5 . . ? 
C16 C15 C14 122.2(2) . . ? 
C16 C15 N4 117.9(3) . . ? 
C14 C15 N4 119.9(3) . . ? 
C15 C16 C11 119.9(3) . . ? 
C15 C16 H16 120.0 . . ? 
C11 C16 H16 120.0 . . ? 
N5 C17 S1 177.8(3) . . ? 
 
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 H3B O1  0.846(10) 2.61(3) 3.138(3) 122(3) 3_576 
O3 H3B O2  0.846(10) 1.995(12) 2.819(3) 164(3) 3_576 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              27.00 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.391 
_refine_diff_density_min   -0.421 
_refine_diff_density_rms    0.062