# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'W. Jones'
'Delia A. Haynes'
'W. Motherwell'
'Andrew Trask'

_publ_contact_author_name        'William Jones'
_publ_contact_author_address     
;
Department of Chemistry
University of Cambridge
Lensfield Road
Cambridge
CB2 1EW
UNITED KINGDOM
;

_publ_contact_author_email       WJ10@CAM.AC.UK

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Screening for Crystalline Salts via Mechanochemistry
;

data_wj0514
_database_code_depnum_ccdc_archive 'CCDC 283624'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'trimethoprim succinate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H19 N4 O3, 0.5(C4 H4 O4)'
_chemical_formula_sum            'C16 H21 N4 O5'
_chemical_formula_weight         349.37

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.343(4)
_cell_length_b                   11.672(2)
_cell_length_c                   16.835(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.95(3)
_cell_angle_gamma                90.00
_cell_volume                     3405.8(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9356
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_reflns_number            14870
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.70
_diffrn_reflns_theta_max         27.51
_reflns_number_total             3897
_reflns_number_gt                3434
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_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^)+(0.0506P)^2^+2.4523P] 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         3897
_refine_ls_number_parameters     233
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1069
_refine_ls_wR_factor_gt          0.1025
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_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
N111 N 0.29611(6) 0.98822(10) 0.21961(6) 0.0239(2) Uani 1 1 d . . .
H1N H 0.3142(10) 0.9737(15) 0.1692(11) 0.043(5) Uiso 1 1 d . . .
N112 N 0.31582(6) 0.97591(9) 0.35859(6) 0.0223(2) Uani 1 1 d . . .
N113 N 0.40637(6) 0.90648(10) 0.27488(6) 0.0274(2) Uani 1 1 d . . .
H11A H 0.4351 0.8851 0.3164 0.033 Uiso 1 1 calc R . .
H11B H 0.4223 0.8940 0.2266 0.033 Uiso 1 1 calc R . .
N114 N 0.22877(6) 1.04699(10) 0.44287(6) 0.0260(2) Uani 1 1 d . . .
H11C H 0.2599 1.0249 0.4823 0.031 Uiso 1 1 calc R . .
H11D H 0.1850 1.0812 0.4529 0.031 Uiso 1 1 calc R . .
C111 C 0.33912(6) 0.95759(10) 0.28517(7) 0.0209(2) Uani 1 1 d . . .
C112 C 0.24797(6) 1.02869(10) 0.36832(7) 0.0203(2) Uani 1 1 d . . .
C113 C 0.22728(7) 1.04261(11) 0.22902(7) 0.0240(3) Uani 1 1 d . . .
H113 H 0.1976 1.0648 0.1831 0.029 Uiso 1 1 calc R . .
C114 C 0.19993(6) 1.06597(10) 0.30156(7) 0.0213(2) Uani 1 1 d . . .
C115 C 0.12459(7) 1.12688(11) 0.31210(7) 0.0243(3) Uani 1 1 d . . .
H11E H 0.1061 1.1570 0.2599 0.029 Uiso 1 1 calc R . .
H11F H 0.1337 1.1932 0.3479 0.029 Uiso 1 1 calc R . .
C116 C 0.06147(6) 1.05257(10) 0.34598(7) 0.0209(2) Uani 1 1 d . . .
C117 C 0.00043(6) 1.10537(10) 0.38323(7) 0.0216(2) Uani 1 1 d . . .
H117 H -0.0010 1.1864 0.3883 0.026 Uiso 1 1 calc R . .
C118 C -0.05842(6) 1.03872(11) 0.41288(7) 0.0219(2) Uani 1 1 d . . .
C119 C -0.05613(7) 0.91922(11) 0.40712(7) 0.0234(3) Uani 1 1 d . . .
C120 C 0.00513(7) 0.86763(10) 0.36928(7) 0.0232(2) Uani 1 1 d . . .
C121 C 0.06345(7) 0.93437(11) 0.33846(7) 0.0231(2) Uani 1 1 d . . .
H121 H 0.1048 0.8988 0.3122 0.028 Uiso 1 1 calc R . .
O122 O -0.12189(5) 1.08154(8) 0.44887(6) 0.0296(2) Uani 1 1 d . . .
O123 O -0.11181(6) 0.85626(8) 0.44426(6) 0.0340(2) Uani 1 1 d . . .
O124 O 0.00338(6) 0.75029(8) 0.36588(6) 0.0327(2) Uani 1 1 d . . .
C122 C -0.12552(8) 1.20254(12) 0.45972(9) 0.0370(3) Uani 1 1 d . . .
H12A H -0.0791 1.2286 0.4893 0.055 Uiso 1 1 calc R . .
H12B H -0.1713 1.2218 0.4896 0.055 Uiso 1 1 calc R . .
H12C H -0.1286 1.2404 0.4077 0.055 Uiso 1 1 calc R . .
C123 C -0.16205(8) 0.79007(13) 0.39332(10) 0.0394(3) Uani 1 1 d . . .
H12D H -0.1751 0.8340 0.3451 0.059 Uiso 1 1 calc R . .
H12E H -0.2093 0.7721 0.4210 0.059 Uiso 1 1 calc R . .
H12F H -0.1362 0.7188 0.3789 0.059 Uiso 1 1 calc R . .
C124 C 0.06566(9) 0.69426(12) 0.32857(9) 0.0361(3) Uani 1 1 d . . .
H12G H 0.0709 0.7250 0.2748 0.054 Uiso 1 1 calc R . .
H12H H 0.0553 0.6118 0.3255 0.054 Uiso 1 1 calc R . .
H12I H 0.1136 0.7075 0.3597 0.054 Uiso 1 1 calc R . .
C21 C 0.41979(6) 0.94135(10) 0.06773(7) 0.0210(2) Uani 1 1 d . . .
C22 C 0.45901(7) 0.97931(12) -0.00696(7) 0.0266(3) Uani 1 1 d . . .
H22A H 0.4592 0.9143 -0.0448 0.032 Uiso 1 1 calc R . .
H22B H 0.4283 1.0418 -0.0321 0.032 Uiso 1 1 calc R . .
O21 O 0.34813(5) 0.96142(9) 0.07255(5) 0.0314(2) Uani 1 1 d . . .
O22 O 0.45955(5) 0.89265(8) 0.12148(5) 0.0248(2) 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
N111 0.0186(5) 0.0363(6) 0.0171(5) -0.0002(4) 0.0029(4) -0.0008(4)
N112 0.0180(5) 0.0306(5) 0.0186(5) 0.0002(4) 0.0020(4) -0.0011(4)
N113 0.0206(5) 0.0411(6) 0.0205(5) -0.0015(4) 0.0025(4) 0.0048(4)
N114 0.0203(5) 0.0375(6) 0.0204(5) -0.0011(4) 0.0040(4) 0.0005(4)
C111 0.0179(5) 0.0252(6) 0.0195(5) -0.0003(4) 0.0019(4) -0.0035(4)
C112 0.0175(5) 0.0230(6) 0.0207(5) -0.0001(4) 0.0030(4) -0.0053(4)
C113 0.0184(5) 0.0320(6) 0.0217(6) 0.0038(5) -0.0006(4) -0.0026(5)
C114 0.0164(5) 0.0238(6) 0.0239(6) 0.0023(4) 0.0024(4) -0.0030(4)
C115 0.0192(5) 0.0244(6) 0.0293(6) 0.0043(5) 0.0038(5) -0.0001(4)
C116 0.0162(5) 0.0253(6) 0.0213(5) 0.0025(4) 0.0002(4) -0.0006(4)
C117 0.0198(5) 0.0208(5) 0.0242(6) 0.0013(4) 0.0013(4) 0.0000(4)
C118 0.0178(5) 0.0274(6) 0.0204(5) -0.0016(4) 0.0019(4) 0.0006(4)
C119 0.0208(5) 0.0266(6) 0.0230(6) 0.0003(5) 0.0036(4) -0.0054(5)
C120 0.0235(6) 0.0212(6) 0.0249(6) 0.0003(4) 0.0016(4) -0.0012(4)
C121 0.0189(5) 0.0249(6) 0.0255(6) 0.0007(5) 0.0035(4) 0.0014(4)
O122 0.0232(4) 0.0304(5) 0.0359(5) -0.0040(4) 0.0120(4) 0.0001(4)
O123 0.0338(5) 0.0333(5) 0.0358(5) -0.0051(4) 0.0153(4) -0.0147(4)
O124 0.0353(5) 0.0208(5) 0.0427(5) -0.0005(4) 0.0125(4) -0.0010(4)
C122 0.0340(7) 0.0323(7) 0.0454(8) -0.0071(6) 0.0113(6) 0.0062(6)
C123 0.0285(7) 0.0348(8) 0.0551(9) -0.0024(7) 0.0040(6) -0.0113(6)
C124 0.0411(8) 0.0248(7) 0.0429(8) -0.0010(6) 0.0094(6) 0.0059(6)
C21 0.0193(5) 0.0267(6) 0.0172(5) -0.0044(4) 0.0020(4) -0.0035(4)
C22 0.0196(6) 0.0431(7) 0.0173(5) 0.0013(5) 0.0017(4) -0.0034(5)
O21 0.0177(4) 0.0579(7) 0.0186(4) -0.0001(4) 0.0028(3) 0.0019(4)
O22 0.0227(4) 0.0309(5) 0.0210(4) 0.0033(3) 0.0028(3) 0.0009(3)

_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
N111 C111 1.3589(16) . ?
N111 C113 1.3660(16) . ?
N111 H1N 0.930(19) . ?
N112 C111 1.3307(15) . ?
N112 C112 1.3432(15) . ?
N113 C111 1.3265(16) . ?
N113 H11A 0.8800 . ?
N113 H11B 0.8800 . ?
N114 C112 1.3267(16) . ?
N114 H11C 0.8800 . ?
N114 H11D 0.8800 . ?
C112 C114 1.4432(17) . ?
C113 C114 1.3526(17) . ?
C113 H113 0.9500 . ?
C114 C115 1.5033(16) . ?
C115 C116 1.5226(16) . ?
C115 H11E 0.9900 . ?
C115 H11F 0.9900 . ?
C116 C121 1.3860(17) . ?
C116 C117 1.3924(17) . ?
C117 C118 1.3895(17) . ?
C117 H117 0.9500 . ?
C118 O122 1.3689(14) . ?
C118 C119 1.3988(18) . ?
C119 O123 1.3799(14) . ?
C119 C120 1.3940(17) . ?
C120 O124 1.3711(15) . ?
C120 C121 1.3909(17) . ?
C121 H121 0.9500 . ?
O122 C122 1.4257(17) . ?
O123 C123 1.4286(17) . ?
O124 C124 1.4266(16) . ?
C122 H12A 0.9800 . ?
C122 H12B 0.9800 . ?
C122 H12C 0.9800 . ?
C123 H12D 0.9800 . ?
C123 H12E 0.9800 . ?
C123 H12F 0.9800 . ?
C124 H12G 0.9800 . ?
C124 H12H 0.9800 . ?
C124 H12I 0.9800 . ?
C21 O22 1.2551(15) . ?
C21 O21 1.2700(14) . ?
C21 C22 1.5159(16) . ?
C22 C22 1.512(2) 5_675 ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?

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
C111 N111 C113 119.07(10) . . ?
C111 N111 H1N 120.1(11) . . ?
C113 N111 H1N 120.9(11) . . ?
C111 N112 C112 118.81(10) . . ?
C111 N113 H11A 120.0 . . ?
C111 N113 H11B 120.0 . . ?
H11A N113 H11B 120.0 . . ?
C112 N114 H11C 120.0 . . ?
C112 N114 H11D 120.0 . . ?
H11C N114 H11D 120.0 . . ?
N113 C111 N112 119.32(11) . . ?
N113 C111 N111 118.23(11) . . ?
N112 C111 N111 122.44(11) . . ?
N114 C112 N112 115.99(11) . . ?
N114 C112 C114 122.10(11) . . ?
N112 C112 C114 121.89(10) . . ?
C114 C113 N111 122.20(11) . . ?
C114 C113 H113 118.9 . . ?
N111 C113 H113 118.9 . . ?
C113 C114 C112 115.56(11) . . ?
C113 C114 C115 122.32(11) . . ?
C112 C114 C115 122.12(10) . . ?
C114 C115 C116 114.43(10) . . ?
C114 C115 H11E 108.7 . . ?
C116 C115 H11E 108.7 . . ?
C114 C115 H11F 108.7 . . ?
C116 C115 H11F 108.7 . . ?
H11E C115 H11F 107.6 . . ?
C121 C116 C117 120.21(11) . . ?
C121 C116 C115 120.83(10) . . ?
C117 C116 C115 118.93(11) . . ?
C118 C117 C116 119.53(11) . . ?
C118 C117 H117 120.2 . . ?
C116 C117 H117 120.2 . . ?
O122 C118 C117 124.47(11) . . ?
O122 C118 C119 114.83(10) . . ?
C117 C118 C119 120.70(11) . . ?
O123 C119 C120 122.20(11) . . ?
O123 C119 C118 118.54(11) . . ?
C120 C119 C118 119.09(11) . . ?
O124 C120 C121 124.00(11) . . ?
O124 C120 C119 115.75(10) . . ?
C121 C120 C119 120.24(11) . . ?
C116 C121 C120 120.20(11) . . ?
C116 C121 H121 119.9 . . ?
C120 C121 H121 119.9 . . ?
C118 O122 C122 117.27(10) . . ?
C119 O123 C123 115.97(10) . . ?
C120 O124 C124 117.41(10) . . ?
O122 C122 H12A 109.5 . . ?
O122 C122 H12B 109.5 . . ?
H12A C122 H12B 109.5 . . ?
O122 C122 H12C 109.5 . . ?
H12A C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
O123 C123 H12D 109.5 . . ?
O123 C123 H12E 109.5 . . ?
H12D C123 H12E 109.5 . . ?
O123 C123 H12F 109.5 . . ?
H12D C123 H12F 109.5 . . ?
H12E C123 H12F 109.5 . . ?
O124 C124 H12G 109.5 . . ?
O124 C124 H12H 109.5 . . ?
H12G C124 H12H 109.5 . . ?
O124 C124 H12I 109.5 . . ?
H12G C124 H12I 109.5 . . ?
H12H C124 H12I 109.5 . . ?
O22 C21 O21 123.53(11) . . ?
O22 C21 C22 118.65(10) . . ?
O21 C21 C22 117.82(11) . . ?
C22 C22 C21 114.26(12) 5_675 . ?
C22 C22 H22A 108.7 5_675 . ?
C21 C22 H22A 108.7 . . ?
C22 C22 H22B 108.7 5_675 . ?
C21 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?

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
C112 N112 C111 N113 179.39(11) . . . . ?
C112 N112 C111 N111 -1.37(17) . . . . ?
C113 N111 C111 N113 -178.95(11) . . . . ?
C113 N111 C111 N112 1.80(18) . . . . ?
C111 N112 C112 N114 -178.42(11) . . . . ?
C111 N112 C112 C114 -0.06(17) . . . . ?
C111 N111 C113 C114 -0.78(18) . . . . ?
N111 C113 C114 C112 -0.54(17) . . . . ?
N111 C113 C114 C115 179.37(11) . . . . ?
N114 C112 C114 C113 179.24(11) . . . . ?
N112 C112 C114 C113 0.98(17) . . . . ?
N114 C112 C114 C115 -0.66(18) . . . . ?
N112 C112 C114 C115 -178.92(11) . . . . ?
C113 C114 C115 C116 111.40(13) . . . . ?
C112 C114 C115 C116 -68.70(15) . . . . ?
C114 C115 C116 C121 -23.33(16) . . . . ?
C114 C115 C116 C117 158.14(11) . . . . ?
C121 C116 C117 C118 0.07(17) . . . . ?
C115 C116 C117 C118 178.61(10) . . . . ?
C116 C117 C118 O122 -178.44(11) . . . . ?
C116 C117 C118 C119 1.32(17) . . . . ?
O122 C118 C119 O123 -6.52(16) . . . . ?
C117 C118 C119 O123 173.70(11) . . . . ?
O122 C118 C119 C120 178.12(11) . . . . ?
C117 C118 C119 C120 -1.66(17) . . . . ?
O123 C119 C120 O124 4.87(17) . . . . ?
C118 C119 C120 O124 -179.95(11) . . . . ?
O123 C119 C120 C121 -174.55(11) . . . . ?
C118 C119 C120 C121 0.64(18) . . . . ?
C117 C116 C121 C120 -1.09(17) . . . . ?
C115 C116 C121 C120 -179.60(11) . . . . ?
O124 C120 C121 C116 -178.64(11) . . . . ?
C119 C120 C121 C116 0.73(18) . . . . ?
C117 C118 O122 C122 -3.09(18) . . . . ?
C119 C118 O122 C122 177.14(11) . . . . ?
C120 C119 O123 C123 -68.20(16) . . . . ?
C118 C119 O123 C123 116.59(13) . . . . ?
C121 C120 O124 C124 0.23(18) . . . . ?
C119 C120 O124 C124 -179.16(11) . . . . ?
O22 C21 C22 C22 -35.1(2) . . . 5_675 ?
O21 C21 C22 C22 144.49(15) . . . 5_675 ?

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
N111 H1N O21 0.930(19) 1.75(2) 2.6820(15) 174.2(17) .

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.042