# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_author_name                'Zhenhui Kang'
_publ_contact_author_email       zhanglili19880330@126.com

data_1
_database_code_depnum_ccdc_archive 'CCDC 880520'
#TrackingRef '- 1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Na(H2O)4][V18O42(VO4)](H2O)16'
_chemical_formula_sum            'H40 Na O66 V19'
_chemical_formula_weight         2087.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4/m

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

_cell_length_a                   13.3146(10)
_cell_length_b                   13.3146(10)
_cell_length_c                   15.876(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2814.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9227
_cell_measurement_theta_min      3.060
_cell_measurement_theta_max      28.288

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2032
_exptl_absorpt_coefficient_mu    3.133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5081
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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 APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18536
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0087
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1284
_reflns_number_gt                1219
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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.
Even though some residual electron densities were observed, they were not
included in the structural model because of the difficulties in the explanation
of the chemical sense.
;

_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^)+(0.0608P)^2^+61.8067P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1284
_refine_ls_number_parameters     113
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1592
_refine_ls_wR_factor_gt          0.1575
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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
V1 V 0.0000 1.0000 0.0000 0.0455(10) Uani 1 8 d S . .
V2 V 0.28660(12) 0.92856(12) 0.0000 0.0296(5) Uani 1 2 d S . .
V3 V 0.13884(12) 0.76822(12) 0.0000 0.0284(4) Uani 1 2 d S . .
V4 V -0.04742(9) 0.81538(8) 0.15999(7) 0.0289(4) Uani 1 1 d . . .
V5 V 0.0000 1.0000 0.24795(14) 0.0283(6) Uani 1 4 d S . .
Na1 Na 0.0000 1.0000 0.5000 0.0345(18) Uani 1 8 d S . .
O1 O 0.0470(7) 0.9203(6) 0.0553(5) 0.0245(19) Uani 0.50 1 d P . .
O2 O 0.4045(5) 0.9004(6) 0.0000 0.046(2) Uani 1 2 d S . .
O3 O 0.2006(6) 0.6651(5) 0.0000 0.047(2) Uani 1 2 d S . .
O4 O -0.0705(5) 0.7323(5) 0.2307(4) 0.0532(16) Uani 1 1 d . . .
O5 O 0.0000 1.0000 0.3495(6) 0.050(3) Uani 1 4 d S . .
O6 O 0.2151(4) 0.8473(4) 0.0796(3) 0.0391(12) Uani 1 1 d . . .
O7 O 0.0330(4) 0.7403(4) 0.0799(3) 0.0416(13) Uani 1 1 d . . .
O8 O 0.0685(4) 0.8847(4) 0.2061(4) 0.0416(13) Uani 1 1 d . . .
O9 O -0.0091(7) 1.1759(6) 0.5000 0.056(2) Uani 1 2 d S . .
H9A H -0.0476 1.2268 0.5000 0.068 Uiso 1 2 d SR . .
H9B H 0.0512 1.1970 0.5000 0.068 Uiso 1 2 d SR . .
O1W O 0.0456(6) 0.4092(6) 0.6459(6) 0.088(3) Uani 1 1 d . . .
H1WA H 0.0539 0.3651 0.6840 0.106 Uiso 1 1 d R . .
H1WB H 0.1029 0.4256 0.6267 0.106 Uiso 1 1 d R . .
O2W O 0.8810(7) 0.2307(7) 0.3563(6) 0.093(3) Uani 1 1 d . . .
H2WA H 0.8257 0.2618 0.3626 0.112 Uiso 1 1 d R . .
H2WB H 0.8812 0.2026 0.3082 0.112 Uiso 1 1 d R . .

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
V1 0.0467(14) 0.0467(14) 0.043(2) 0.000 0.000 0.000
V2 0.0200(8) 0.0296(9) 0.0392(10) 0.000 0.000 0.0020(6)
V3 0.0239(8) 0.0187(8) 0.0425(10) 0.000 0.000 0.0044(6)
V4 0.0355(7) 0.0246(6) 0.0266(7) 0.0073(5) 0.0016(5) -0.0027(4)
V5 0.0343(8) 0.0343(8) 0.0162(11) 0.000 0.000 0.000
Na1 0.037(3) 0.037(3) 0.029(4) 0.000 0.000 0.000
O1 0.025(4) 0.026(4) 0.022(5) 0.001(4) -0.003(4) 0.001(3)
O2 0.023(4) 0.053(5) 0.063(5) 0.000 0.000 0.007(3)
O3 0.038(4) 0.024(4) 0.078(6) 0.000 0.000 0.008(3)
O4 0.069(4) 0.047(3) 0.043(3) 0.023(3) 0.007(3) -0.004(3)
O5 0.069(5) 0.069(5) 0.014(5) 0.000 0.000 0.000
O6 0.042(3) 0.038(3) 0.037(3) -0.008(2) 0.006(2) -0.012(2)
O7 0.029(3) 0.055(3) 0.040(3) -0.012(3) 0.003(2) -0.005(2)
O8 0.036(3) 0.041(3) 0.048(3) -0.009(2) 0.006(2) -0.007(2)
O9 0.042(5) 0.033(4) 0.094(7) 0.000 0.000 -0.002(3)
O1W 0.075(5) 0.074(5) 0.116(7) 0.035(5) 0.016(5) 0.012(4)
O2W 0.105(7) 0.108(7) 0.067(5) -0.011(5) 0.011(5) 0.053(5)

_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
V1 O1 1.513(8) 11_465 ?
V1 O1 1.513(8) 2_575 ?
V1 O1 1.513(8) 3_665 ?
V1 O1 1.513(8) 9_575 ?
V1 O1 1.513(8) 4_465 ?
V1 O1 1.513(8) . ?
V1 O1 1.513(8) 12_665 ?
V1 O1 1.513(8) 10 ?
V2 O2 1.614(7) . ?
V2 O7 1.916(5) 3_665 ?
V2 O7 1.916(5) 12_665 ?
V2 O6 1.917(5) 10 ?
V2 O6 1.917(5) . ?
V2 V3 2.893(2) 3_665 ?
V2 V4 2.8978(15) 12_665 ?
V2 V4 2.8978(15) 3_665 ?
V2 V3 2.903(2) . ?
V3 O3 1.600(7) . ?
V3 O7 1.932(5) 10 ?
V3 O7 1.932(5) . ?
V3 O6 1.933(5) . ?
V3 O6 1.933(5) 10 ?
V3 V2 2.893(2) 11_465 ?
V4 O4 1.605(5) . ?
V4 O8 1.934(5) 4_465 ?
V4 O6 1.938(5) 4_465 ?
V4 O7 1.940(5) . ?
V4 O8 1.942(5) . ?
V4 V5 2.8967(16) . ?
V4 V2 2.8978(15) 11_465 ?
V5 O5 1.613(10) . ?
V5 O8 1.905(5) 4_465 ?
V5 O8 1.905(5) 2_575 ?
V5 O8 1.905(5) . ?
V5 O8 1.905(5) 3_665 ?
V5 V4 2.8967(16) 4_465 ?
V5 V4 2.8967(16) 2_575 ?
V5 V4 2.8967(16) 3_665 ?
Na1 O9 2.345(8) 3_665 ?
Na1 O9 2.345(8) . ?
Na1 O9 2.345(8) 9_576 ?
Na1 O9 2.345(8) 11_466 ?
Na1 O5 2.389(10) . ?
Na1 O5 2.389(10) 9_576 ?
O1 O1 1.743(12) 4_465 ?
O1 O1 1.743(12) 3_665 ?
O1 O1 1.757(17) 10 ?
O6 V4 1.938(5) 3_665 ?
O7 V2 1.916(5) 11_465 ?
O8 V4 1.934(5) 3_665 ?

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 V1 O1 109.7(3) 11_465 2_575 ?
O1 V1 O1 180.000(2) 11_465 3_665 ?
O1 V1 O1 70.3(3) 2_575 3_665 ?
O1 V1 O1 70.3(3) 11_465 9_575 ?
O1 V1 O1 71.0(6) 2_575 9_575 ?
O1 V1 O1 109.7(3) 3_665 9_575 ?
O1 V1 O1 71.0(6) 11_465 4_465 ?
O1 V1 O1 70.3(3) 2_575 4_465 ?
O1 V1 O1 109.0(6) 3_665 4_465 ?
O1 V1 O1 109.7(3) 9_575 4_465 ?
O1 V1 O1 109.7(3) 11_465 . ?
O1 V1 O1 109.0(6) 2_575 . ?
O1 V1 O1 70.3(3) 3_665 . ?
O1 V1 O1 180.0(5) 9_575 . ?
O1 V1 O1 70.3(3) 4_465 . ?
O1 V1 O1 109.0(6) 11_465 12_665 ?
O1 V1 O1 109.7(3) 2_575 12_665 ?
O1 V1 O1 71.0(6) 3_665 12_665 ?
O1 V1 O1 70.3(3) 9_575 12_665 ?
O1 V1 O1 180.000(2) 4_465 12_665 ?
O1 V1 O1 109.7(3) . 12_665 ?
O1 V1 O1 70.3(3) 11_465 10 ?
O1 V1 O1 180.0(5) 2_575 10 ?
O1 V1 O1 109.7(3) 3_665 10 ?
O1 V1 O1 109.0(6) 9_575 10 ?
O1 V1 O1 109.7(3) 4_465 10 ?
O1 V1 O1 71.0(6) . 10 ?
O1 V1 O1 70.3(3) 12_665 10 ?
O2 V2 O7 110.5(3) . 3_665 ?
O2 V2 O7 110.5(3) . 12_665 ?
O7 V2 O7 82.9(3) 3_665 12_665 ?
O2 V2 O6 110.6(3) . 10 ?
O7 V2 O6 138.9(3) 3_665 10 ?
O7 V2 O6 83.1(2) 12_665 10 ?
O2 V2 O6 110.6(3) . . ?
O7 V2 O6 83.1(2) 3_665 . ?
O7 V2 O6 138.9(3) 12_665 . ?
O6 V2 O6 82.5(3) 10 . ?
O2 V2 V3 118.0(3) . 3_665 ?
O7 V2 V3 41.45(16) 3_665 3_665 ?
O7 V2 V3 41.45(16) 12_665 3_665 ?
O6 V2 V3 114.88(17) 10 3_665 ?
O6 V2 V3 114.88(17) . 3_665 ?
O2 V2 V4 118.78(3) . 12_665 ?
O7 V2 V4 114.35(18) 3_665 12_665 ?
O7 V2 V4 41.58(16) 12_665 12_665 ?
O6 V2 V4 41.55(15) 10 12_665 ?
O6 V2 V4 114.05(17) . 12_665 ?
V3 V2 V4 77.00(4) 3_665 12_665 ?
O2 V2 V4 118.78(3) . 3_665 ?
O7 V2 V4 41.58(16) 3_665 3_665 ?
O7 V2 V4 114.35(18) 12_665 3_665 ?
O6 V2 V4 114.05(17) 10 3_665 ?
O6 V2 V4 41.55(15) . 3_665 ?
V3 V2 V4 77.00(4) 3_665 3_665 ?
V4 V2 V4 122.45(7) 12_665 3_665 ?
O2 V2 V3 119.3(3) . . ?
O7 V2 V3 114.01(17) 3_665 . ?
O7 V2 V3 114.01(17) 12_665 . ?
O6 V2 V3 41.27(16) 10 . ?
O6 V2 V3 41.27(16) . . ?
V3 V2 V3 122.73(8) 3_665 . ?
V4 V2 V3 76.33(4) 12_665 . ?
V4 V2 V3 76.33(4) 3_665 . ?
O3 V3 O7 102.1(3) . 10 ?
O3 V3 O7 102.1(3) . . ?
O7 V3 O7 82.1(3) 10 . ?
O3 V3 O6 101.4(3) . . ?
O7 V3 O6 156.5(3) 10 . ?
O7 V3 O6 93.4(2) . . ?
O3 V3 O6 101.4(3) . 10 ?
O7 V3 O6 93.4(2) 10 10 ?
O7 V3 O6 156.5(3) . 10 ?
O6 V3 O6 81.6(3) . 10 ?
O3 V3 V2 106.3(3) . 11_465 ?
O7 V3 V2 41.03(16) 10 11_465 ?
O7 V3 V2 41.03(16) . 11_465 ?
O6 V3 V2 130.22(16) . 11_465 ?
O6 V3 V2 130.22(16) 10 11_465 ?
O3 V3 V2 106.4(3) . . ?
O7 V3 V2 129.47(16) 10 . ?
O7 V3 V2 129.47(16) . . ?
O6 V3 V2 40.84(16) . . ?
O6 V3 V2 40.84(16) 10 . ?
V2 V3 V2 147.27(8) 11_465 . ?
O4 V4 O8 101.3(3) . 4_465 ?
O4 V4 O6 100.2(3) . 4_465 ?
O8 V4 O6 94.5(2) 4_465 4_465 ?
O4 V4 O7 102.1(3) . . ?
O8 V4 O7 156.6(3) 4_465 . ?
O6 V4 O7 81.9(2) 4_465 . ?
O4 V4 O8 102.5(3) . . ?
O8 V4 O8 81.3(3) 4_465 . ?
O6 V4 O8 157.3(2) 4_465 . ?
O7 V4 O8 93.1(2) . . ?
O4 V4 V5 106.8(2) . . ?
O8 V4 V5 40.64(16) 4_465 . ?
O6 V4 V5 130.74(16) 4_465 . ?
O7 V4 V5 129.26(16) . . ?
O8 V4 V5 40.67(16) . . ?
O4 V4 V2 105.6(2) . 11_465 ?
O8 V4 V2 130.90(17) 4_465 11_465 ?
O6 V4 V2 40.98(16) 4_465 11_465 ?
O7 V4 V2 40.97(16) . 11_465 ?
O8 V4 V2 129.87(17) . 11_465 ?
V5 V4 V2 147.59(6) . 11_465 ?
O5 V5 O8 110.40(19) . 4_465 ?
O5 V5 O8 110.40(19) . 2_575 ?
O8 V5 O8 83.02(12) 4_465 2_575 ?
O5 V5 O8 110.40(19) . . ?
O8 V5 O8 83.02(12) 4_465 . ?
O8 V5 O8 139.2(4) 2_575 . ?
O5 V5 O8 110.40(19) . 3_665 ?
O8 V5 O8 139.2(4) 4_465 3_665 ?
O8 V5 O8 83.02(12) 2_575 3_665 ?
O8 V5 O8 83.02(12) . 3_665 ?
O5 V5 V4 118.82(4) . 4_465 ?
O8 V5 V4 41.64(16) 4_465 4_465 ?
O8 V5 V4 41.41(16) 2_575 4_465 ?
O8 V5 V4 114.46(18) . 4_465 ?
O8 V5 V4 114.29(18) 3_665 4_465 ?
O5 V5 V4 118.82(4) . . ?
O8 V5 V4 41.41(16) 4_465 . ?
O8 V5 V4 114.29(18) 2_575 . ?
O8 V5 V4 41.64(16) . . ?
O8 V5 V4 114.46(18) 3_665 . ?
V4 V5 V4 76.56(4) 4_465 . ?
O5 V5 V4 118.82(4) . 2_575 ?
O8 V5 V4 114.46(18) 4_465 2_575 ?
O8 V5 V4 41.64(16) 2_575 2_575 ?
O8 V5 V4 114.29(18) . 2_575 ?
O8 V5 V4 41.41(16) 3_665 2_575 ?
V4 V5 V4 76.56(4) 4_465 2_575 ?
V4 V5 V4 122.36(9) . 2_575 ?
O5 V5 V4 118.82(4) . 3_665 ?
O8 V5 V4 114.29(18) 4_465 3_665 ?
O8 V5 V4 114.46(18) 2_575 3_665 ?
O8 V5 V4 41.41(16) . 3_665 ?
O8 V5 V4 41.64(16) 3_665 3_665 ?
V4 V5 V4 122.36(9) 4_465 3_665 ?
V4 V5 V4 76.56(4) . 3_665 ?
V4 V5 V4 76.56(4) 2_575 3_665 ?
O9 Na1 O9 90.0 3_665 . ?
O9 Na1 O9 90.000(1) 3_665 9_576 ?
O9 Na1 O9 180.000(1) . 9_576 ?
O9 Na1 O9 180.0 3_665 11_466 ?
O9 Na1 O9 90.000(1) . 11_466 ?
O9 Na1 O9 90.000(1) 9_576 11_466 ?
O9 Na1 O5 90.000(1) 3_665 . ?
O9 Na1 O5 90.0 . . ?
O9 Na1 O5 90.0 9_576 . ?
O9 Na1 O5 90.000(1) 11_466 . ?
O9 Na1 O5 90.000(1) 3_665 9_576 ?
O9 Na1 O5 90.0 . 9_576 ?
O9 Na1 O5 90.0 9_576 9_576 ?
O9 Na1 O5 90.000(1) 11_466 9_576 ?
O5 Na1 O5 180.000(1) . 9_576 ?
V1 O1 O1 54.85(16) . 4_465 ?
V1 O1 O1 54.85(16) . 3_665 ?
O1 O1 O1 90.000(1) 4_465 3_665 ?
V1 O1 O1 54.5(3) . 10 ?
O1 O1 O1 90.000(1) 4_465 10 ?
O1 O1 O1 90.0 3_665 10 ?
V5 O5 Na1 180.0 . . ?
V2 O6 V3 97.9(2) . . ?
V2 O6 V4 97.5(2) . 3_665 ?
V3 O6 V4 135.6(3) . 3_665 ?
V2 O7 V3 97.5(2) 11_465 . ?
V2 O7 V4 97.5(2) 11_465 . ?
V3 O7 V4 137.2(3) . . ?
V5 O8 V4 98.0(2) . 3_665 ?
V5 O8 V4 97.7(2) . . ?
V4 O8 V4 135.6(3) 3_665 . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.735
_refine_diff_density_min         -3.269
_refine_diff_density_rms         0.182