Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2003

data_global
_journal_name_full               'J.Chem.Soc.,Dalton Trans.'

_journal_coden_Cambridge         0186

loop_
_publ_author_name
'Enbo Wang'
'Gejihu De'
'Changwen Hu'
'Ning-Hai Hu'
'Rudan Huang'
;
Hengqing Jia
;
'Yangguang Li'
'Mei Yuan'

_publ_contact_author_name        'Prof Enbo Wang'
_publ_contact_author_address     
;
Department of Chemistry 
Institute of Polyoxometalate Chemistry 
Northeast Normal University 
Changchun 
Jilin 
130024 
CHINA 
;

_publ_contact_author_email       WANGENBO@PUBLIC.CC.JL.CN

_publ_section_title              
;
A novel two-dimensional arsenic vanadate network 
grafted with a transition metal complex: [Cu(phen)]2[VIVVV4As2O19]กค0.5H2O 
(phen = o-phenanthroline)
;

data_m062a
_database_code_CSD               188034

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H17 As2 Cu2 N4 O19.50 V5'
_chemical_formula_weight         1205.04

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   11.4154(10)
_cell_length_b                   10.0380(5)
_cell_length_c                   14.8841(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.411(4)
_cell_angle_gamma                90.00
_cell_volume                     1702.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6673
_cell_measurement_theta_min      1.79
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.571
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.185
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_absorpt_coefficient_mu    4.558
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6134
_exptl_absorpt_correction_T_max  1.2120
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6673
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3885
_reflns_number_gt                3287
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_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^)+(0.0806P)^2^+0.0000P] 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         3885
_refine_ls_number_parameters     266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0866
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_restrained_S_all      0.899
_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
Cu Cu -0.22000(3) 0.44061(4) -0.03416(3) 0.01630(11) Uani 1 1 d . . .
V1 V 0.05088(9) 0.00062(11) -0.01648(7) 0.0152(2) Uani 0.50 1 d P . .
V2 V 0.10018(5) 0.07925(5) 0.17725(3) 0.01696(13) Uani 1 1 d . . .
V3 V 0.06718(5) -0.22507(5) 0.17742(3) 0.01699(14) Uani 1 1 d . . .
As As 0.03409(2) 0.32321(3) 0.021638(18) 0.01108(10) Uani 1 1 d . . .
O1 O -0.09371(18) 0.3873(2) 0.05015(14) 0.0165(4) Uani 1 1 d . . .
O2 O 0.0435(2) 0.3124(2) -0.08974(14) 0.0192(5) Uani 1 1 d . . .
O3 O 0.14686(19) 0.3999(2) 0.07404(15) 0.0185(5) Uani 1 1 d . . .
O4 O 0.0401(2) 0.1611(2) 0.06070(14) 0.0167(5) Uani 1 1 d . . .
O5 O 0.0698(2) -0.0716(2) 0.10074(14) 0.0196(5) Uani 1 1 d . . .
O6 O 0.1055(2) -0.0729(2) 0.26045(15) 0.0216(5) Uani 1 1 d . . .
O7 O 0.1722(4) 0.0025(6) -0.0637(4) 0.0323(12) Uani 0.50 1 d P . .
O8 O 0.2330(3) 0.1283(3) 0.1815(2) 0.0479(9) Uani 1 1 d . . .
O9 O -0.0191(4) -0.3175(3) 0.26201(17) 0.0505(10) Uani 1 1 d . . .
O10 O 0.1875(3) -0.3040(3) 0.16788(18) 0.0340(6) Uani 1 1 d . . .
N1 N -0.3667(2) 0.4899(3) -0.10711(18) 0.0201(6) Uani 1 1 d . . .
N2 N -0.3266(2) 0.3025(3) 0.0151(2) 0.0238(6) Uani 1 1 d . . .
C1 C -0.3817(3) 0.5856(4) -0.1678(2) 0.0256(7) Uani 1 1 d . . .
H1 H -0.3188 0.6404 -0.1798 0.026 Uiso 1 1 calc R . .
C2 C -0.4906(3) 0.6059(4) -0.2145(3) 0.0325(9) Uani 1 1 d . . .
H2 H -0.4991 0.6727 -0.2577 0.033 Uiso 1 1 calc R . .
C3 C -0.5847(3) 0.5272(4) -0.1965(3) 0.0328(9) Uani 1 1 d . . .
H3 H -0.6575 0.5419 -0.2261 0.033 Uiso 1 1 calc R . .
C4 C -0.5701(3) 0.4246(4) -0.1331(2) 0.0256(8) Uani 1 1 d . . .
C5 C -0.4585(3) 0.4092(3) -0.0904(2) 0.0191(6) Uani 1 1 d . . .
C6 C -0.4367(3) 0.3091(4) -0.0236(2) 0.0229(7) Uani 1 1 d . . .
C7 C -0.5285(3) 0.2249(4) 0.0005(3) 0.0287(8) Uani 1 1 d . . .
C8 C -0.5005(4) 0.1299(4) 0.0688(3) 0.0399(10) Uani 1 1 d . . .
H8 H -0.5578 0.0721 0.0876 0.040 Uiso 1 1 calc R . .
C9 C -0.3893(4) 0.1237(5) 0.1066(3) 0.0426(11) Uani 1 1 d . . .
H9 H -0.3697 0.0607 0.1508 0.043 Uiso 1 1 calc R . .
C10 C -0.3038(4) 0.2135(4) 0.0785(3) 0.0379(10) Uani 1 1 d . . .
H10 H -0.2285 0.2095 0.1058 0.038 Uiso 1 1 calc R . .
C11 C -0.6616(3) 0.3370(4) -0.1067(3) 0.0329(9) Uani 1 1 d . . .
H11 H -0.7367 0.3461 -0.1339 0.033 Uiso 1 1 calc R . .
C12 C -0.6415(3) 0.2430(5) -0.0443(3) 0.0359(9) Uani 1 1 d . . .
H12 H -0.7028 0.1878 -0.0295 0.036 Uiso 1 1 calc R . .
OW O 0.1557(11) 0.0757(13) -0.2104(8) 0.040(3) Uiso 0.25 1 d P . .

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
Cu 0.0138(2) 0.0147(2) 0.0201(2) 0.00210(15) -0.00188(14) -0.00202(14)
V1 0.0207(5) 0.0125(5) 0.0125(5) -0.0002(4) 0.0011(4) -0.0003(4)
V2 0.0261(3) 0.0104(3) 0.0137(3) 0.0000(2) -0.0046(2) 0.0005(2)
V3 0.0297(3) 0.0102(3) 0.0107(2) 0.00089(19) -0.0014(2) 0.0022(2)
As 0.01427(16) 0.00854(16) 0.01033(15) 0.00065(10) 0.00000(11) -0.00034(10)
O1 0.0138(10) 0.0190(12) 0.0166(10) -0.0019(9) -0.0002(8) 0.0038(8)
O2 0.0296(13) 0.0169(12) 0.0111(9) 0.0006(9) 0.0025(9) -0.0028(9)
O3 0.0193(11) 0.0149(12) 0.0207(11) 0.0029(9) -0.0041(9) -0.0056(9)
O4 0.0310(13) 0.0074(11) 0.0111(10) 0.0011(8) -0.0024(8) 0.0010(8)
O5 0.0348(13) 0.0136(11) 0.0098(10) 0.0019(8) -0.0032(9) -0.0003(9)
O6 0.0385(14) 0.0146(12) 0.0115(10) 0.0008(8) -0.0007(9) -0.0009(10)
O7 0.027(3) 0.030(3) 0.041(3) -0.008(3) 0.012(2) -0.006(2)
O8 0.0381(17) 0.0409(18) 0.061(2) 0.0287(16) -0.0291(14) -0.0191(14)
O9 0.107(3) 0.0322(17) 0.0143(12) -0.0069(11) 0.0168(15) -0.0403(17)
O10 0.0379(16) 0.0302(15) 0.0327(14) -0.0073(12) -0.0086(12) 0.0154(12)
N1 0.0184(13) 0.0193(15) 0.0225(13) -0.0026(11) -0.0009(11) -0.0013(11)
N2 0.0190(14) 0.0231(15) 0.0291(15) 0.0045(12) -0.0002(11) -0.0045(11)
C1 0.0284(18) 0.0224(19) 0.0251(17) 0.0015(14) -0.0064(14) 0.0003(14)
C2 0.033(2) 0.034(2) 0.0291(18) 0.0007(17) -0.0118(15) 0.0019(16)
C3 0.0253(19) 0.040(2) 0.0322(18) -0.0082(18) -0.0100(15) 0.0048(16)
C4 0.0171(16) 0.030(2) 0.0288(18) -0.0117(15) -0.0024(13) -0.0004(14)
C5 0.0161(15) 0.0186(16) 0.0226(15) -0.0079(13) 0.0004(12) -0.0022(12)
C6 0.0182(16) 0.0226(18) 0.0282(17) -0.0068(14) 0.0041(13) -0.0056(13)
C7 0.0248(18) 0.028(2) 0.0337(18) -0.0040(16) 0.0090(14) -0.0080(14)
C8 0.034(2) 0.033(2) 0.054(3) 0.005(2) 0.0152(18) -0.0157(18)
C9 0.039(2) 0.037(2) 0.053(3) 0.022(2) 0.0059(19) -0.0097(19)
C10 0.033(2) 0.036(2) 0.044(2) 0.0142(19) -0.0020(18) -0.0082(17)
C11 0.0153(16) 0.045(3) 0.038(2) -0.0152(19) 0.0002(14) -0.0064(15)
C12 0.0195(18) 0.042(2) 0.047(2) -0.015(2) 0.0095(16) -0.0127(17)

_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
Cu O3 1.916(2) 3_565 ?
Cu O1 1.930(2) . ?
Cu N1 2.003(3) . ?
Cu N2 2.012(3) . ?
V1 V1 1.288(2) 3 ?
V1 O7 1.590(5) . ?
V1 O5 1.890(2) . ?
V1 O5 1.942(2) 3 ?
V1 O4 1.987(2) . ?
V1 O4 2.016(2) 3 ?
V1 V2 2.9752(11) 3 ?
V1 V2 3.0102(11) . ?
V2 O8 1.592(3) . ?
V2 O9 1.688(3) 2 ?
V2 O5 1.914(2) . ?
V2 O6 1.965(2) . ?
V2 O4 2.003(2) . ?
V2 V1 2.9752(11) 3 ?
V2 V3 3.0780(8) . ?
V3 O10 1.599(3) . ?
V3 O9 1.888(3) . ?
V3 O5 1.919(2) . ?
V3 O2 1.967(2) 3 ?
V3 O6 1.997(2) . ?
As O3 1.655(2) . ?
As O2 1.671(2) . ?
As O1 1.672(2) . ?
As O4 1.728(2) . ?
O2 V3 1.967(2) 3 ?
O3 Cu 1.916(2) 3_565 ?
O4 V1 2.016(2) 3 ?
O5 V1 1.942(2) 3 ?
O9 V2 1.688(3) 2_545 ?
N1 C1 1.323(5) . ?
N1 C5 1.360(4) . ?
N2 C10 1.314(5) . ?
N2 C6 1.353(4) . ?
C1 C2 1.403(5) . ?
C2 C3 1.372(6) . ?
C3 C4 1.400(6) . ?
C4 C5 1.398(5) . ?
C4 C11 1.438(5) . ?
C5 C6 1.425(5) . ?
C6 C7 1.409(5) . ?
C7 C8 1.416(6) . ?
C7 C12 1.428(6) . ?
C8 C9 1.359(6) . ?
C9 C10 1.410(6) . ?
C11 C12 1.335(6) . ?

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
O3 Cu O1 96.35(9) 3_565 . ?
O3 Cu N1 89.49(11) 3_565 . ?
O1 Cu N1 171.56(10) . . ?
O3 Cu N2 166.64(11) 3_565 . ?
O1 Cu N2 90.95(11) . . ?
N1 Cu N2 82.17(12) . . ?
V1 V1 O7 176.2(2) 3 . ?
V1 V1 O5 72.58(11) 3 . ?
O7 V1 O5 111.0(2) . . ?
V1 V1 O5 68.18(11) 3 3 ?
O7 V1 O5 108.3(2) . 3 ?
O5 V1 O5 140.76(7) . 3 ?
V1 V1 O4 72.50(11) 3 . ?
O7 V1 O4 109.3(2) . . ?
O5 V1 O4 77.56(10) . . ?
O5 V1 O4 90.58(10) 3 . ?
V1 V1 O4 69.99(11) 3 3 ?
O7 V1 O4 108.1(2) . 3 ?
O5 V1 O4 91.21(10) . 3 ?
O5 V1 O4 75.68(10) 3 3 ?
O4 V1 O4 142.48(7) . 3 ?
V1 V1 V2 79.11(9) 3 3 ?
O7 V1 V2 97.26(19) . 3 ?
O5 V1 V2 131.93(9) . 3 ?
O5 V1 V2 39.15(7) 3 3 ?
O4 V1 V2 129.11(8) . 3 ?
O4 V1 V2 42.09(6) 3 3 ?
V1 V1 V2 76.06(8) 3 . ?
O7 V1 V2 107.57(19) . . ?
O5 V1 V2 37.96(7) . . ?
O5 V1 V2 127.40(8) 3 . ?
O4 V1 V2 41.23(6) . . ?
O4 V1 V2 125.95(8) 3 . ?
V2 V1 V2 155.16(4) 3 . ?
O8 V2 O9 109.9(2) . 2 ?
O8 V2 O5 114.03(16) . . ?
O9 V2 O5 135.97(16) 2 . ?
O8 V2 O6 102.80(13) . . ?
O9 V2 O6 97.89(12) 2 . ?
O5 V2 O6 76.00(9) . . ?
O8 V2 O4 100.59(13) . . ?
O9 V2 O4 92.38(11) 2 . ?
O5 V2 O4 76.61(9) . . ?
O6 V2 O4 149.41(10) . . ?
O8 V2 V1 128.36(13) . 3 ?
O9 V2 V1 106.64(13) 2 3 ?
O5 V2 V1 39.85(7) . 3 ?
O6 V2 V1 107.00(7) . 3 ?
O4 V2 V1 42.43(7) . 3 ?
O8 V2 V1 104.05(13) . . ?
O9 V2 V1 126.66(12) 2 . ?
O5 V2 V1 37.40(7) . . ?
O6 V2 V1 113.39(7) . . ?
O4 V2 V1 40.81(6) . . ?
V1 V2 V1 24.84(4) 3 . ?
O8 V2 V3 115.05(13) . . ?
O9 V2 V3 122.56(13) 2 . ?
O5 V2 V3 36.63(6) . . ?
O6 V2 V3 39.41(7) . . ?
O4 V2 V3 111.85(6) . . ?
V1 V2 V3 70.62(3) 3 . ?
V1 V2 V3 74.02(3) . . ?
O10 V3 O9 107.50(17) . . ?
O10 V3 O5 107.54(14) . . ?
O9 V3 O5 144.93(15) . . ?
O10 V3 O2 103.95(12) . 3 ?
O9 V3 O2 83.32(12) . 3 ?
O5 V3 O2 89.72(9) . 3 ?
O10 V3 O6 106.04(13) . . ?
O9 V3 O6 93.85(10) . . ?
O5 V3 O6 75.12(9) . . ?
O2 V3 O6 149.28(11) 3 . ?
O10 V3 V2 112.71(11) . . ?
O9 V3 V2 123.84(10) . . ?
O5 V3 V2 36.51(7) . . ?
O2 V3 V2 121.02(7) 3 . ?
O6 V3 V2 38.64(6) . . ?
O3 As O2 113.83(11) . . ?
O3 As O1 111.55(11) . . ?
O2 As O1 112.65(11) . . ?
O3 As O4 105.37(11) . . ?
O2 As O4 105.60(10) . . ?
O1 As O4 107.15(11) . . ?
As O1 Cu 124.82(12) . . ?
As O2 V3 127.64(13) . 3 ?
As O3 Cu 125.71(12) . 3_565 ?
As O4 V1 124.86(11) . . ?
As O4 V2 133.02(12) . . ?
V1 O4 V2 97.96(10) . . ?
As O4 V1 129.71(12) . 3 ?
V1 O4 V1 37.52(7) . 3 ?
V2 O4 V1 95.49(9) . 3 ?
V1 O5 V2 104.65(11) . . ?
V1 O5 V3 148.44(13) . . ?
V2 O5 V3 106.85(10) . . ?
V1 O5 V1 39.24(7) . 3 ?
V2 O5 V1 101.00(11) . 3 ?
V3 O5 V1 130.02(13) . 3 ?
V2 O6 V3 101.95(10) . . ?
V2 O9 V3 169.63(17) 2_545 . ?
C1 N1 C5 119.2(3) . . ?
C1 N1 Cu 128.3(2) . . ?
C5 N1 Cu 112.5(2) . . ?
C10 N2 C6 118.5(3) . . ?
C10 N2 Cu 129.2(3) . . ?
C6 N2 Cu 112.2(2) . . ?
N1 C1 C2 121.3(4) . . ?
C3 C2 C1 120.0(4) . . ?
C2 C3 C4 119.5(3) . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 C11 117.7(4) . . ?
C3 C4 C11 125.1(3) . . ?
N1 C5 C4 122.8(3) . . ?
N1 C5 C6 116.3(3) . . ?
C4 C5 C6 120.8(3) . . ?
N2 C6 C7 123.3(3) . . ?
N2 C6 C5 116.8(3) . . ?
C7 C6 C5 119.9(3) . . ?
C6 C7 C8 116.5(3) . . ?
C6 C7 C12 118.0(4) . . ?
C8 C7 C12 125.5(4) . . ?
C9 C8 C7 119.6(4) . . ?
C8 C9 C10 119.5(4) . . ?
N2 C10 C9 122.5(4) . . ?
C12 C11 C4 121.7(4) . . ?
C11 C12 C7 121.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.269