 
data_06skc0075p-1
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
Pyrrolidinium tri-aniline-2-sulphonate
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C22 H30 N4 O9 S3'
_chemical_formula_weight          590.68
 
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'
 'S'  'S'   0.1246   0.1234
 '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                    10.0617(6)
_cell_length_b                    10.7224(6)
_cell_length_c                    12.7612(8)
_cell_angle_alpha                 90.665(3)
_cell_angle_beta                  105.835(3)
_cell_angle_gamma                 99.831(3)
_cell_volume                      1302.59(13)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     5583
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.14
_exptl_crystal_size_mid           0.09
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.506
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              620
_exptl_absorpt_coefficient_mu     0.344
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9535
_exptl_absorpt_correction_T_max   0.9932
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             33410
_diffrn_reflns_av_R_equivalents   0.1208
_diffrn_reflns_av_sigmaI/netI     0.0957
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          3.05
_diffrn_reflns_theta_max          27.48
_reflns_number_total              5944
_reflns_number_gt                 3976
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'  
_computing_structure_solution     ?
_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)+(0.0000P)²+6.8153P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5944
_refine_ls_number_parameters      345
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1441
_refine_ls_R_factor_gt            0.0848
_refine_ls_wR_factor_ref          0.1711
_refine_ls_wR_factor_gt           0.1455
_refine_ls_goodness_of_fit_ref    1.101
_refine_ls_restrained_S_all       1.101
_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
C1 C 0.2967(5) 0.1112(4) 0.1694(4) 0.0231(10) Uani 1 1 d . . .
C2 C 0.3915(5) 0.0350(4) 0.2250(4) 0.0221(10) Uani 1 1 d . . .
C3 C 0.4231(5) -0.0602(5) 0.1638(4) 0.0278(11) Uani 1 1 d . . .
H3 H 0.4863 -0.1130 0.1996 0.033 Uiso 1 1 calc R . .
C4 C 0.3638(6) -0.0776(5) 0.0531(5) 0.0372(14) Uani 1 1 d . . .
H4 H 0.3860 -0.1427 0.0133 0.045 Uiso 1 1 calc R . .
C5 C 0.2724(7) -0.0021(5) -0.0013(4) 0.0432(16) Uani 1 1 d . . .
H5 H 0.2323 -0.0144 -0.0781 0.052 Uiso 1 1 calc R . .
C6 C 0.2401(6) 0.0913(5) 0.0572(4) 0.0335(13) Uani 1 1 d . . .
H6 H 0.1774 0.1435 0.0198 0.040 Uiso 1 1 calc R . .
N2 N 0.4437(4) 0.0452(4) 0.3380(3) 0.0236(9) Uani 1 1 d . . .
H2A H 0.4967 -0.0078 0.3713 0.028 Uiso 1 1 calc R . .
H2B H 0.4239 0.1048 0.3761 0.028 Uiso 1 1 calc R . .
O1A O 0.1609(4) 0.1621(3) 0.3050(3) 0.0280(8) Uani 1 1 d . . .
O1B O 0.1669(4) 0.3016(3) 0.1578(3) 0.0340(9) Uani 1 1 d . . .
O1C O 0.3738(3) 0.3039(3) 0.3098(3) 0.0261(8) Uani 1 1 d . . .
S1 S 0.24572(12) 0.22990(10) 0.23936(9) 0.0192(3) Uani 1 1 d . . .
C22 C 0.9860(6) 0.3814(5) 0.3538(5) 0.0341(13) Uani 1 1 d . . .
H22A H 1.0735 0.3960 0.3308 0.041 Uiso 1 1 calc R . .
H22B H 1.0089 0.4088 0.4321 0.041 Uiso 1 1 calc R . .
C23 C 0.8783(7) 0.4527(5) 0.2850(6) 0.0480(17) Uani 1 1 d . . .
H23A H 0.8130 0.4734 0.3255 0.058 Uiso 1 1 calc R . .
H23B H 0.9242 0.5319 0.2608 0.058 Uiso 1 1 calc R . .
C24 C 0.8041(10) 0.3598(8) 0.1908(6) 0.082(3) Uani 1 1 d . . .
H24A H 0.7105 0.3792 0.1536 0.098 Uiso 1 1 calc R . .
H24B H 0.8594 0.3610 0.1373 0.098 Uiso 1 1 calc R . .
C25 C 0.7903(8) 0.2345(6) 0.2394(6) 0.066(2) Uani 1 1 d . . .
H25A H 0.7875 0.1657 0.1860 0.080 Uiso 1 1 calc R . .
H25B H 0.7037 0.2172 0.2635 0.080 Uiso 1 1 calc R . .
N21 N 0.9172(4) 0.2449(4) 0.3341(3) 0.0228(9) Uani 1 1 d . . .
H21A H 0.9781 0.1967 0.3194 0.027 Uiso 1 1 calc R . .
H21B H 0.8922 0.2161 0.3949 0.027 Uiso 1 1 calc R . .
C31 C 0.2116(5) 0.6961(4) 0.3068(4) 0.0189(9) Uani 1 1 d . . .
C32 C 0.1529(5) 0.8038(4) 0.2776(4) 0.0197(10) Uani 1 1 d . . .
C33 C 0.0763(5) 0.8167(4) 0.1723(4) 0.0227(10) Uani 1 1 d . . .
H33 H 0.0336 0.8890 0.1542 0.027 Uiso 1 1 calc R . .
C34 C 0.0626(5) 0.7212(5) 0.0925(4) 0.0291(12) Uani 1 1 d . . .
H34 H 0.0104 0.7285 0.0193 0.035 Uiso 1 1 calc R . .
C35 C 0.1250(5) 0.6162(5) 0.1201(4) 0.0260(11) Uani 1 1 d . . .
H35 H 0.1171 0.5524 0.0654 0.031 Uiso 1 1 calc R . .
C36 C 0.1992(5) 0.6033(4) 0.2275(4) 0.0232(10) Uani 1 1 d . . .
H36 H 0.2412 0.5307 0.2460 0.028 Uiso 1 1 calc R . .
N32 N 0.1750(4) 0.9082(3) 0.3604(3) 0.0183(8) Uani 1 1 d . . .
H32A H 0.2659 0.9492 0.3775 0.027 Uiso 1 1 calc R . .
H32B H 0.1558 0.8762 0.4215 0.027 Uiso 1 1 calc R . .
H32C H 0.1169 0.9637 0.3334 0.027 Uiso 1 1 calc R . .
O31A O 0.4282(3) 0.7811(3) 0.4675(3) 0.0234(7) Uani 1 1 d . . .
O31B O 0.3396(4) 0.5552(3) 0.4502(3) 0.0276(8) Uani 1 1 d . . .
O31C O 0.2091(4) 0.7018(4) 0.5069(3) 0.0345(9) Uani 1 1 d . . .
S31 S 0.30396(13) 0.68107(10) 0.44454(10) 0.0205(3) Uani 1 1 d . . .
C41 C 0.7179(5) 0.7613(4) 0.3023(4) 0.0189(9) Uani 1 1 d . . .
C42 C 0.6478(5) 0.6719(4) 0.3556(4) 0.0186(9) Uani 1 1 d . . .
C43 C 0.5566(5) 0.5669(4) 0.2989(4) 0.0220(10) Uani 1 1 d . . .
H43 H 0.5113 0.5049 0.3365 0.026 Uiso 1 1 calc R . .
C44 C 0.5315(5) 0.5522(5) 0.1874(4) 0.0285(11) Uani 1 1 d . . .
H44 H 0.4656 0.4818 0.1478 0.034 Uiso 1 1 calc R . .
C45 C 0.6015(5) 0.6394(5) 0.1327(4) 0.0297(12) Uani 1 1 d . . .
H45 H 0.5860 0.6278 0.0561 0.036 Uiso 1 1 calc R . .
C46 C 0.6951(5) 0.7444(5) 0.1912(4) 0.0236(10) Uani 1 1 d . . .
H46 H 0.7434 0.8047 0.1541 0.028 Uiso 1 1 calc R . .
N42 N 0.6663(4) 0.6875(3) 0.4726(3) 0.0210(8) Uani 1 1 d . . .
H42A H 0.7511 0.7372 0.5049 0.031 Uiso 1 1 calc R . .
H42B H 0.6627 0.6103 0.5015 0.031 Uiso 1 1 calc R . .
H42C H 0.5966 0.7250 0.4846 0.031 Uiso 1 1 calc R . .
O41A O 0.8948(3) 0.9661(3) 0.2979(3) 0.0226(7) Uani 1 1 d . . .
O41B O 0.9346(3) 0.8465(3) 0.4617(3) 0.0235(7) Uani 1 1 d . . .
O41C O 0.7458(3) 0.9679(3) 0.4195(3) 0.0248(7) Uani 1 1 d . . .
S41 S 0.83349(12) 0.89859(10) 0.37603(9) 0.0182(3) Uani 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
C1 C6 1.389(7) . ?
C1 C2 1.410(7) . ?
C1 S1 1.768(5) . ?
C2 N2 1.389(6) . ?
C2 C3 1.407(6) . ?
C3 C4 1.372(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.375(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
O1A S1 1.467(3) . ?
O1B S1 1.442(3) . ?
O1C S1 1.449(3) . ?
C22 N21 1.495(6) . ?
C22 C23 1.520(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.491(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.486(10) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 N21 1.487(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
N21 H21A 0.9200 . ?
N21 H21B 0.9200 . ?
C31 C36 1.376(6) . ?
C31 C32 1.394(6) . ?
C31 S31 1.774(5) . ?
C32 C33 1.377(6) . ?
C32 N32 1.477(6) . ?
C33 C34 1.398(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.391(7) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
N32 H32A 0.9100 . ?
N32 H32B 0.9100 . ?
N32 H32C 0.9100 . ?
O31A S31 1.461(3) . ?
O31B S31 1.452(3) . ?
O31C S31 1.441(4) . ?
C41 C46 1.379(6) . ?
C41 C42 1.387(6) . ?
C41 S41 1.786(5) . ?
C42 C43 1.378(6) . ?
C42 N42 1.458(6) . ?
C43 C44 1.377(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.395(7) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
N42 H42A 0.9100 . ?
N42 H42B 0.9100 . ?
N42 H42C 0.9100 . ?
O41A S41 1.449(3) . ?
O41B S41 1.464(3) . ?
O41C S41 1.456(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
C6 C1 C2 119.3(4) . . ?
C6 C1 S1 119.0(4) . . ?
C2 C1 S1 121.7(4) . . ?
N2 C2 C3 120.1(4) . . ?
N2 C2 C1 121.6(4) . . ?
C3 C2 C1 118.2(4) . . ?
C4 C3 C2 120.7(5) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 121.1(5) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 119.0(5) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C1 121.8(5) . . ?
C5 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
C2 N2 H2A 120.0 . . ?
C2 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
O1B S1 O1C 113.9(2) . . ?
O1B S1 O1A 112.7(2) . . ?
O1C S1 O1A 110.2(2) . . ?
O1B S1 C1 107.2(2) . . ?
O1C S1 C1 106.6(2) . . ?
O1A S1 C1 105.7(2) . . ?
N21 C22 C23 104.8(4) . . ?
N21 C22 H22A 110.8 . . ?
C23 C22 H22A 110.8 . . ?
N21 C22 H22B 110.8 . . ?
C23 C22 H22B 110.8 . . ?
H22A C22 H22B 108.9 . . ?
C24 C23 C22 102.3(5) . . ?
C24 C23 H23A 111.3 . . ?
C22 C23 H23A 111.3 . . ?
C24 C23 H23B 111.3 . . ?
C22 C23 H23B 111.3 . . ?
H23A C23 H23B 109.2 . . ?
C25 C24 C23 104.9(6) . . ?
C25 C24 H24A 110.8 . . ?
C23 C24 H24A 110.8 . . ?
C25 C24 H24B 110.8 . . ?
C23 C24 H24B 110.8 . . ?
H24A C24 H24B 108.8 . . ?
C24 C25 N21 104.8(6) . . ?
C24 C25 H25A 110.8 . . ?
N21 C25 H25A 110.8 . . ?
C24 C25 H25B 110.8 . . ?
N21 C25 H25B 110.8 . . ?
H25A C25 H25B 108.9 . . ?
C25 N21 C22 107.9(4) . . ?
C25 N21 H21A 110.1 . . ?
C22 N21 H21A 110.1 . . ?
C25 N21 H21B 110.1 . . ?
C22 N21 H21B 110.1 . . ?
H21A N21 H21B 108.4 . . ?
C36 C31 C32 119.4(4) . . ?
C36 C31 S31 120.7(4) . . ?
C32 C31 S31 120.0(3) . . ?
C33 C32 C31 121.6(4) . . ?
C33 C32 N32 118.6(4) . . ?
C31 C32 N32 119.8(4) . . ?
C32 C33 C34 118.6(4) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 H33 120.7 . . ?
C35 C34 C33 120.0(5) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.5(4) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C31 C36 C35 119.8(4) . . ?
C31 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C32 N32 H32A 109.5 . . ?
C32 N32 H32B 109.5 . . ?
H32A N32 H32B 109.5 . . ?
C32 N32 H32C 109.5 . . ?
H32A N32 H32C 109.5 . . ?
H32B N32 H32C 109.5 . . ?
O31C S31 O31B 114.5(2) . . ?
O31C S31 O31A 112.3(2) . . ?
O31B S31 O31A 112.3(2) . . ?
O31C S31 C31 105.1(2) . . ?
O31B S31 C31 106.6(2) . . ?
O31A S31 C31 105.1(2) . . ?
C46 C41 C42 119.2(4) . . ?
C46 C41 S41 120.2(4) . . ?
C42 C41 S41 120.6(3) . . ?
C43 C42 C41 120.9(4) . . ?
C43 C42 N42 118.1(4) . . ?
C41 C42 N42 121.0(4) . . ?
C44 C43 C42 119.7(5) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C45 120.5(5) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C44 C45 C46 119.3(5) . . ?
C44 C45 H45 120.3 . . ?
C46 C45 H45 120.3 . . ?
C41 C46 C45 120.4(5) . . ?
C41 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C42 N42 H42A 109.5 . . ?
C42 N42 H42B 109.5 . . ?
H42A N42 H42B 109.5 . . ?
C42 N42 H42C 109.5 . . ?
H42A N42 H42C 109.5 . . ?
H42B N42 H42C 109.5 . . ?
O41A S41 O41C 113.99(19) . . ?
O41A S41 O41B 113.8(2) . . ?
O41C S41 O41B 112.5(2) . . ?
O41A S41 C41 106.0(2) . . ?
O41C S41 C41 105.5(2) . . ?
O41B S41 C41 103.8(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
N42 H42C O31A  0.91 1.85 2.737(5) 163.1 .
N42 H42C S31  0.91 2.80 3.553(4) 140.6 .
N2 H2B O1C  0.88 2.39 2.978(5) 124.6 .
N32 H32B O31C  0.91 2.24 2.918(5) 130.3 .
N42 H42A O41B  0.91 2.22 2.976(5) 140.3 .
N42 H42A S41  0.91 2.59 3.061(4) 112.9 .
N2 H2A O41C  0.88 2.47 3.188(5) 138.8 1_545
N21 H21A O41A  0.92 2.46 2.980(5) 116.1 1_545
N2 H2B O31A  0.88 2.32 2.935(5) 126.8 2_666
N21 H21B O31C  0.92 2.09 2.773(5) 130.1 2_666
N42 H42A O1A  0.91 2.51 3.149(5) 128.1 2_666
N42 H42B O31B  0.91 1.88 2.791(5) 174.5 2_666
N21 H21A O1A  0.92 1.99 2.858(5) 156.2 1_655
N21 H21B O41B  0.92 2.35 2.901(5) 118.2 2_766
N32 H32A N2  0.91 2.10 2.937(6) 153.3 1_565
N32 H32C O1A  0.91 2.15 2.837(5) 131.4 1_565
N32 H32B O41B  0.91 2.39 3.022(5) 126.8 1_455
N32 H32C O41A  0.91 2.16 2.890(5) 136.6 1_455
N32 H32C S41  0.91 3.02 3.480(4) 113.5 1_455
N32 H32B O41C  0.91 2.48 2.936(5) 111.2 2_676
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.642
_refine_diff_density_min   -0.576
_refine_diff_density_rms    0.110
