data_global

_publ_contact_author
;
  Shishkina S.V.
  Institute for Single Crystals
  60 Lenina ave.
  Kharkiv, 61072
  Ukraine
;
_publ_contact_author_phone   '380 57 341 02 58'
_publ_contact_author_fax     '380 57 341 02 73'
_publ_contact_author_email   sveta@xray.isc.kharkov.com

_publ_requested_journal      'test'

_publ_contact_letter
;
 Paper containing this structure has been
submitted to Beilstein Journal of Organic Chemistry.
;

_iucr_compatibility_tag       ACTA95

_publ_section_title
;
 The regioselective synthesis of spirooxindolo pyrrolidines and 
pyrrolizidines via three-component reactions of acrylamides and 
aroylacrylic acids with isatins and α-amino acids.
;
loop_
 _publ_author_name
    'Pavlovskaya T.L.'
    'Yaremenko F.G.'
    'Lipson V.V.'
    'Shishkina S.V.'
    'Shishkin O.V.'
    'Musatov V.I.'
    'Karpenko A.S.'
    
_publ_section_exptl_prep
;
?
;

data_experimental 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C20 H15 Br Cl2 N2 O4, C H4 O' 
_chemical_formula_sum 
 'C21 H19 Br Cl2 N2 O5' 
_chemical_formula_weight          530.19 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.2901   2.4595 
 '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                    8.8751(7) 
_cell_length_b                    10.5764(9) 
_cell_length_c                    12.3519(10) 
_cell_angle_alpha                 75.858(5) 
_cell_angle_beta                  84.297(5) 
_cell_angle_gamma                 76.237(5) 
_cell_volume                      1090.96(15) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     466(2) 
_cell_measurement_reflns_used     9455
_cell_measurement_theta_min       2.9 
_cell_measurement_theta_max       32.1 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.614 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              536 
_exptl_absorpt_coefficient_mu     2.165 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.5628 
_exptl_absorpt_correction_T_max   0.6713 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       466(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Enhance (Mo) X-ray Source' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   "Xcalibur"3" 
_diffrn_measurement_method        'ω-scans' 
_diffrn_detector_area_resol_mean  16.1827 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             15210 
_diffrn_reflns_av_R_equivalents   0.0430 
_diffrn_reflns_av_sigmaI/netI     0.0499 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          1.70 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3801 
_reflns_number_gt                 2435 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection         
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;         
_computing_cell_refinement         
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_reduction          
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_structure_solution     'SHELXTL (Sheldrick, 1998)' 
_computing_structure_refinement   'SHELXTL (Sheldrick, 1998)' 
_computing_molecular_graphics     'XP (Siemens, 1998)'  
_computing_publication_material   'SHELXTL (Sheldrick, 1998)' 
 
_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)+(0.0528P)²+0.1236P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    difmap 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3801 
_refine_ls_number_parameters      284 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0820 
_refine_ls_R_factor_gt            0.0430 
_refine_ls_wR_factor_ref          0.1103 
_refine_ls_wR_factor_gt           0.1012 
_refine_ls_goodness_of_fit_ref    1.055 
_refine_ls_restrained_S_all       1.055 
_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 
Br1 Br 0.84201(6) 0.29747(5) 0.91508(4) 0.0912(2) Uani 1 1 d . . . 
Cl1 Cl 0.72426(12) 0.91348(12) 1.02543(9) 0.0803(4) Uani 1 1 d . . . 
Cl2 Cl 0.61990(14) 0.63795(13) 1.09429(8) 0.0852(4) Uani 1 1 d . . . 
O1 O 0.7071(2) 0.9108(2) 0.4247(2) 0.0505(6) Uani 1 1 d . . . 
O2 O 0.1705(2) 0.8714(2) 0.5173(2) 0.0535(6) Uani 1 1 d . . . 
O3 O 0.2167(3) 0.8053(3) 0.3589(2) 0.0660(8) Uani 1 1 d . . . 
H3O H 0.1288 0.8510 0.3469 0.099 Uiso 1 1 calc R . . 
O4 O 0.3585(3) 0.6365(2) 0.72939(18) 0.0523(6) Uani 1 1 d . . . 
N1 N 0.8572(3) 0.8091(3) 0.5757(2) 0.0436(7) Uani 1 1 d . . . 
H1N H 0.9154 0.8655 0.5677 0.052 Uiso 1 1 calc R . . 
N2 N 0.6646(3) 0.6245(2) 0.4672(2) 0.0333(6) Uani 1 1 d . . . 
C1 C 0.8700(3) 0.6932(3) 0.6616(3) 0.0382(8) Uani 1 1 d . . . 
C2 C 0.9706(4) 0.6480(4) 0.7480(3) 0.0520(9) Uani 1 1 d . . . 
H2 H 1.0434 0.6954 0.7554 0.062 Uiso 1 1 calc R . . 
C3 C 0.9592(4) 0.5302(4) 0.8232(3) 0.0572(10) Uani 1 1 d . . . 
H3 H 1.0235 0.4985 0.8835 0.069 Uiso 1 1 calc R . . 
C4 C 0.8545(4) 0.4589(3) 0.8101(3) 0.0484(9) Uani 1 1 d . . . 
C5 C 0.7551(3) 0.5033(3) 0.7216(3) 0.0395(8) Uani 1 1 d . . . 
H5 H 0.6863 0.4534 0.7120 0.047 Uiso 1 1 calc R . . 
C6 C 0.7619(3) 0.6228(3) 0.6491(2) 0.0319(7) Uani 1 1 d . . . 
C7 C 0.6646(3) 0.7018(3) 0.5500(2) 0.0291(7) Uani 1 1 d . . . 
C8 C 0.7432(3) 0.8215(3) 0.5076(3) 0.0344(7) Uani 1 1 d . . . 
C9 C 0.4868(3) 0.7578(3) 0.5750(2) 0.0265(6) Uani 1 1 d . . . 
H9 H 0.4662 0.8556 0.5534 0.032 Uiso 1 1 calc R . . 
C10 C 0.4041(3) 0.7095(3) 0.4946(2) 0.0301(7) Uani 1 1 d . . . 
H10 H 0.3809 0.6235 0.5340 0.036 Uiso 1 1 calc R . . 
C11 C 0.5254(3) 0.6842(3) 0.4032(3) 0.0349(7) Uani 1 1 d . . . 
H11B H 0.5023 0.6230 0.3634 0.042 Uiso 1 1 calc R . . 
H11A H 0.5353 0.7667 0.3505 0.042 Uiso 1 1 calc R . . 
C12 C 0.8067(4) 0.6006(4) 0.3993(3) 0.0549(10) Uani 1 1 d . . . 
H12C H 0.8919 0.5560 0.4469 0.082 Uiso 1 1 calc R . . 
H12B H 0.8256 0.6844 0.3559 0.082 Uiso 1 1 calc R . . 
H12A H 0.7968 0.5456 0.3502 0.082 Uiso 1 1 calc R . . 
C13 C 0.2532(3) 0.8044(3) 0.4586(3) 0.0338(7) Uani 1 1 d . . . 
C14 C 0.4394(3) 0.7175(3) 0.6971(3) 0.0338(7) Uani 1 1 d . . . 
C15 C 0.5010(3) 0.7742(3) 0.7783(2) 0.0352(7) Uani 1 1 d . . . 
C16 C 0.5475(3) 0.8956(3) 0.7486(3) 0.0409(8) Uani 1 1 d . . . 
H16 H 0.5338 0.9482 0.6765 0.049 Uiso 1 1 calc R . . 
C17 C 0.6137(4) 0.9374(3) 0.8259(3) 0.0497(9) Uani 1 1 d . . . 
H17 H 0.6428 1.0192 0.8062 0.060 Uiso 1 1 calc R . . 
C18 C 0.6368(4) 0.8600(4) 0.9311(3) 0.0479(9) Uani 1 1 d . . . 
C19 C 0.5895(4) 0.7406(4) 0.9626(3) 0.0490(9) Uani 1 1 d . . . 
C20 C 0.5201(4) 0.6991(3) 0.8860(3) 0.0453(8) Uani 1 1 d . . . 
H20 H 0.4861 0.6196 0.9075 0.054 Uiso 1 1 calc R . . 
O1S O -0.0300(3) 0.9994(3) 0.3012(2) 0.0668(7) Uani 1 1 d . . . 
H1OS H -0.0919 0.9622 0.3432 0.100 Uiso 1 1 calc R . . 
C1S C -0.0773(5) 1.0311(5) 0.1930(3) 0.0816(14) Uani 1 1 d . . . 
H1SC H -0.1359 1.1218 0.1754 0.122 Uiso 1 1 calc R . . 
H1SB H -0.1411 0.9722 0.1857 0.122 Uiso 1 1 calc R . . 
H1SA H 0.0121 1.0213 0.1426 0.122 Uiso 1 1 calc R . . 
 
 
_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 
Br1 C4 1.894(3) . ? 
Cl1 C18 1.730(3) . ? 
Cl2 C19 1.727(3) . ? 
O1 C8 1.222(4) . ? 
O2 C13 1.210(4) . ? 
O3 C13 1.301(4) . ? 
O4 C14 1.215(3) . ? 
N1 C8 1.343(4) . ? 
N1 C1 1.401(4) . ? 
N2 C12 1.449(4) . ? 
N2 C7 1.456(4) . ? 
N2 C11 1.459(4) . ? 
C1 C2 1.379(4) . ? 
C1 C6 1.387(4) . ? 
C2 C3 1.379(5) . ? 
C3 C4 1.371(5) . ? 
C4 C5 1.392(4) . ? 
C5 C6 1.369(4) . ? 
C6 C7 1.519(4) . ? 
C7 C8 1.545(4) . ? 
C7 C9 1.576(4) . ? 
C9 C14 1.509(4) . ? 
C9 C10 1.535(4) . ? 
C10 C13 1.503(4) . ? 
C10 C11 1.508(4) . ? 
C14 C15 1.492(4) . ? 
C15 C20 1.376(4) . ? 
C15 C16 1.395(4) . ? 
C16 C17 1.377(4) . ? 
C17 C18 1.361(5) . ? 
C18 C19 1.379(5) . ? 
C19 C20 1.384(5) . ? 
O1S C1S 1.378(4) . ? 
 
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 
C8 N1 C1 111.8(2) . . ? 
C12 N2 C7 115.9(2) . . ? 
C12 N2 C11 114.2(2) . . ? 
C7 N2 C11 108.1(2) . . ? 
C2 C1 C6 121.8(3) . . ? 
C2 C1 N1 128.7(3) . . ? 
C6 C1 N1 109.5(2) . . ? 
C3 C2 C1 117.6(3) . . ? 
C4 C3 C2 120.9(3) . . ? 
C3 C4 C5 121.4(3) . . ? 
C3 C4 Br1 119.7(3) . . ? 
C5 C4 Br1 118.9(3) . . ? 
C6 C5 C4 118.0(3) . . ? 
C5 C6 C1 120.3(3) . . ? 
C5 C6 C7 130.9(2) . . ? 
C1 C6 C7 108.8(2) . . ? 
N2 C7 C6 112.9(2) . . ? 
N2 C7 C8 114.0(2) . . ? 
C6 C7 C8 101.1(2) . . ? 
N2 C7 C9 103.6(2) . . ? 
C6 C7 C9 117.2(2) . . ? 
C8 C7 C9 108.4(2) . . ? 
O1 C8 N1 126.5(3) . . ? 
O1 C8 C7 124.8(2) . . ? 
N1 C8 C7 108.7(3) . . ? 
C14 C9 C10 115.6(2) . . ? 
C14 C9 C7 112.6(2) . . ? 
C10 C9 C7 104.1(2) . . ? 
C13 C10 C11 116.5(2) . . ? 
C13 C10 C9 112.3(2) . . ? 
C11 C10 C9 104.1(2) . . ? 
N2 C11 C10 101.4(2) . . ? 
O2 C13 O3 122.6(3) . . ? 
O2 C13 C10 123.7(3) . . ? 
O3 C13 C10 113.7(3) . . ? 
O4 C14 C15 120.5(3) . . ? 
O4 C14 C9 121.1(3) . . ? 
C15 C14 C9 118.4(2) . . ? 
C20 C15 C16 118.9(3) . . ? 
C20 C15 C14 117.9(3) . . ? 
C16 C15 C14 123.1(3) . . ? 
C17 C16 C15 120.0(3) . . ? 
C18 C17 C16 120.5(3) . . ? 
C17 C18 C19 120.4(3) . . ? 
C17 C18 Cl1 119.4(3) . . ? 
C19 C18 Cl1 120.2(3) . . ? 
C18 C19 C20 119.5(3) . . ? 
C18 C19 Cl2 121.8(3) . . ? 
C20 C19 Cl2 118.7(3) . . ? 
C15 C20 C19 120.7(3) . . ? 
 
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 
C8 N1 C1 C2 -178.7(3) . . . . ? 
C8 N1 C1 C6 1.4(4) . . . . ? 
C6 C1 C2 C3 -0.6(5) . . . . ? 
N1 C1 C2 C3 179.5(3) . . . . ? 
C1 C2 C3 C4 1.8(5) . . . . ? 
C2 C3 C4 C5 -0.6(5) . . . . ? 
C2 C3 C4 Br1 -179.9(3) . . . . ? 
C3 C4 C5 C6 -1.8(5) . . . . ? 
Br1 C4 C5 C6 177.5(2) . . . . ? 
C4 C5 C6 C1 2.9(4) . . . . ? 
C4 C5 C6 C7 -175.9(3) . . . . ? 
C2 C1 C6 C5 -1.8(5) . . . . ? 
N1 C1 C6 C5 178.1(3) . . . . ? 
C2 C1 C6 C7 177.3(3) . . . . ? 
N1 C1 C6 C7 -2.8(3) . . . . ? 
C12 N2 C7 C6 -73.4(3) . . . . ? 
C11 N2 C7 C6 157.0(2) . . . . ? 
C12 N2 C7 C8 41.2(3) . . . . ? 
C11 N2 C7 C8 -88.4(3) . . . . ? 
C12 N2 C7 C9 158.8(2) . . . . ? 
C11 N2 C7 C9 29.2(3) . . . . ? 
C5 C6 C7 N2 -55.9(4) . . . . ? 
C1 C6 C7 N2 125.1(3) . . . . ? 
C5 C6 C7 C8 -178.1(3) . . . . ? 
C1 C6 C7 C8 2.9(3) . . . . ? 
C5 C6 C7 C9 64.4(4) . . . . ? 
C1 C6 C7 C9 -114.6(3) . . . . ? 
C1 N1 C8 O1 -178.6(3) . . . . ? 
C1 N1 C8 C7 0.6(3) . . . . ? 
N2 C7 C8 O1 55.7(4) . . . . ? 
C6 C7 C8 O1 177.1(3) . . . . ? 
C9 C7 C8 O1 -59.2(4) . . . . ? 
N2 C7 C8 N1 -123.5(3) . . . . ? 
C6 C7 C8 N1 -2.1(3) . . . . ? 
C9 C7 C8 N1 121.6(3) . . . . ? 
N2 C7 C9 C14 122.7(2) . . . . ? 
C6 C7 C9 C14 -2.4(3) . . . . ? 
C8 C7 C9 C14 -115.9(3) . . . . ? 
N2 C7 C9 C10 -3.2(3) . . . . ? 
C6 C7 C9 C10 -128.3(2) . . . . ? 
C8 C7 C9 C10 118.2(2) . . . . ? 
C14 C9 C10 C13 86.8(3) . . . . ? 
C7 C9 C10 C13 -149.2(2) . . . . ? 
C14 C9 C10 C11 -146.3(2) . . . . ? 
C7 C9 C10 C11 -22.3(3) . . . . ? 
C12 N2 C11 C10 -174.2(2) . . . . ? 
C7 N2 C11 C10 -43.7(3) . . . . ? 
C13 C10 C11 N2 163.8(2) . . . . ? 
C9 C10 C11 N2 39.5(3) . . . . ? 
C11 C10 C13 O2 -152.1(3) . . . . ? 
C9 C10 C13 O2 -32.1(4) . . . . ? 
C11 C10 C13 O3 29.8(4) . . . . ? 
C9 C10 C13 O3 149.7(3) . . . . ? 
C10 C9 C14 O4 10.2(4) . . . . ? 
C7 C9 C14 O4 -109.2(3) . . . . ? 
C10 C9 C14 C15 -172.9(2) . . . . ? 
C7 C9 C14 C15 67.7(3) . . . . ? 
O4 C14 C15 C20 25.9(4) . . . . ? 
C9 C14 C15 C20 -151.0(3) . . . . ? 
O4 C14 C15 C16 -157.6(3) . . . . ? 
C9 C14 C15 C16 25.4(4) . . . . ? 
C20 C15 C16 C17 1.1(5) . . . . ? 
C14 C15 C16 C17 -175.3(3) . . . . ? 
C15 C16 C17 C18 1.2(5) . . . . ? 
C16 C17 C18 C19 -2.2(5) . . . . ? 
C16 C17 C18 Cl1 178.5(2) . . . . ? 
C17 C18 C19 C20 0.9(5) . . . . ? 
Cl1 C18 C19 C20 -179.8(3) . . . . ? 
C17 C18 C19 Cl2 178.7(3) . . . . ? 
Cl1 C18 C19 Cl2 -2.0(4) . . . . ? 
C16 C15 C20 C19 -2.3(5) . . . . ? 
C14 C15 C20 C19 174.2(3) . . . . ? 
C18 C19 C20 C15 1.4(5) . . . . ? 
Cl2 C19 C20 C15 -176.5(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 H3O O1S  0.82 1.86 2.641(3) 159.9 . 
N1 H1N O2  0.86 2.30 2.988(3) 137.2 1_655 
O1S H1OS O1  0.82 2.08 2.878(3) 164.2 1_455 
 
_diffrn_measured_fraction_theta_max    0.989 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.989 
_refine_diff_density_max    0.493 
_refine_diff_density_min   -0.493 
_refine_diff_density_rms    0.056 
