# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global

_journal_coden_Cambridge         222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Philip Lightfoot'
'Phoebe Allan'
'Richard J. Goff'
'Farida A. Himeur'
'Russell E. Morris'
'Simon J. Teat'

_publ_contact_author_name        'Philip Lightfoot'
_publ_contact_author_email       PL@ST-ANDREWS.AC.UK

_publ_section_title              
;
Increasing the dimensionality
of hybrid vanadium oxyfluorides using ionothermal synthesis
;

# Attachment 'Himeur.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 761277'
#TrackingRef 'Himeur.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H6 F5 N O2 V2'
_chemical_formula_weight         308.99

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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   7.5691(7)
_cell_length_b                   19.912(2)
_cell_length_c                   11.9888(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.436(2)
_cell_angle_gamma                90.00
_cell_volume                     1806.4(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    14039
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      30.5

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_absorpt_coefficient_mu    2.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         '11.3.1 ALS. LBNL. Calif.'
_diffrn_radiation_monochromator  'Si(111) Crystal'
_diffrn_measurement_device_type  'Bruker AXS APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            15416
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         33.57
_reflns_number_total             5354
_reflns_number_gt                3447
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEXII (Bruker, 2006)'
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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^)+(0.0397P)^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         5354
_refine_ls_number_parameters     279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0881
_refine_ls_wR_factor_gt          0.0765
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_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
V1 V 0.95859(5) 0.19185(2) 0.87517(3) 0.01006(9) Uani 1 1 d . . .
V2 V 1.44772(5) 0.18876(2) 0.56393(3) 0.01044(9) Uani 1 1 d . . .
V3 V 0.95758(5) 0.18822(2) 0.56428(3) 0.01024(9) Uani 1 1 d . . .
V4 V 1.44736(5) 0.19220(2) 0.87402(3) 0.00997(9) Uani 1 1 d . . .
F8 F 1.49517(19) 0.21394(8) 0.71900(11) 0.0161(3) Uani 1 1 d . . .
F10 F 1.42240(18) 0.20736(7) 1.03277(11) 0.0134(3) Uani 1 1 d . . .
F5 F 0.91106(18) 0.21242(8) 0.71786(11) 0.0149(3) Uani 1 1 d . . .
F9 F 0.98829(18) 0.20004(7) 0.40219(11) 0.0131(3) Uani 1 1 d . . .
O3 O 0.9923(2) 0.10905(10) 0.56872(15) 0.0173(4) Uani 1 1 d . . .
O2 O 1.4181(2) 0.10967(10) 0.56899(15) 0.0182(4) Uani 1 1 d . . .
O1 O 0.9921(2) 0.11314(10) 0.87203(15) 0.0181(4) Uani 1 1 d . . .
O4 O 1.4103(2) 0.11371(10) 0.86775(15) 0.0177(4) Uani 1 1 d . . .
F4 F 1.20137(17) 0.22322(8) 0.84927(12) 0.0137(3) Uani 1 1 d . . .
F2 F 0.98925(18) 0.20724(7) 1.03456(11) 0.0131(3) Uani 1 1 d . . .
F6 F 1.20347(17) 0.21660(8) 0.58821(11) 0.0148(3) Uani 1 1 d . . .
F3 F 0.91723(18) 0.29874(7) 0.90197(11) 0.0131(3) Uani 1 1 d . . .
F7 F 1.70207(18) 0.18336(8) 0.53730(12) 0.0147(3) Uani 1 1 d . . .
F1 F 0.70358(17) 0.18793(8) 0.89850(12) 0.0149(3) Uani 1 1 d . . .
N1 N 1.1749(3) 0.10562(13) 0.3001(2) 0.0212(5) Uani 1 1 d . . .
N2 N 1.1752(3) 0.37305(15) 0.7944(2) 0.0297(6) Uani 1 1 d . . .
C5 C 1.2203(3) 0.11929(15) 0.1950(2) 0.0232(6) Uani 1 1 d . . .
H5 H 1.2067 0.1634 0.1658 0.028 Uiso 1 1 calc R . .
C7 C 1.2829(4) 0.41554(15) 0.6267(3) 0.0260(6) Uani 1 1 d . . .
H7 H 1.3157 0.4092 0.5515 0.031 Uiso 1 1 calc R . .
C6 C 1.2204(4) 0.36287(15) 0.6868(3) 0.0251(6) Uani 1 1 d . . .
H6 H 1.2087 0.3197 0.6539 0.030 Uiso 1 1 calc R . .
C4 C 1.2870(4) 0.06865(17) 0.1301(2) 0.0253(6) Uani 1 1 d . . .
H4 H 1.3199 0.0774 0.0555 0.030 Uiso 1 1 calc R . .
C2 C 1.2574(4) -0.00754(15) 0.2840(3) 0.0259(6) Uani 1 1 d . . .
H2 H 1.2700 -0.0512 0.3152 0.031 Uiso 1 1 calc R . .
C3 C 1.3055(4) 0.00508(16) 0.1747(3) 0.0258(6) Uani 1 1 d . . .
H3 H 1.3512 -0.0302 0.1305 0.031 Uiso 1 1 calc R . .
C8 C 1.2983(4) 0.47780(15) 0.6753(3) 0.0263(6) Uani 1 1 d . . .
H8 H 1.3428 0.5145 0.6338 0.032 Uiso 1 1 calc R . .
C9 C 1.2490(4) 0.48729(16) 0.7849(3) 0.0281(7) Uani 1 1 d . . .
H9 H 1.2577 0.5303 0.8189 0.034 Uiso 1 1 calc R . .
C1 C 1.1914(4) 0.04429(16) 0.3458(2) 0.0242(6) Uani 1 1 d . . .
H1 H 1.1575 0.0368 0.4206 0.029 Uiso 1 1 calc R . .
C10 C 1.1875(4) 0.43299(18) 0.8429(3) 0.0304(7) Uani 1 1 d . . .
H10 H 1.1534 0.4383 0.9182 0.037 Uiso 1 1 calc R . .
H21 H 1.124(5) 0.333(2) 0.828(3) 0.061(13) Uiso 1 1 d . . .
H11 H 1.125(5) 0.139(2) 0.338(3) 0.057(13) Uiso 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
V1 0.00891(18) 0.0138(2) 0.00753(18) -0.00007(16) 0.00056(14) 0.00048(15)
V2 0.00929(18) 0.0146(2) 0.00750(18) 0.00083(16) 0.00070(14) -0.00043(15)
V3 0.00871(18) 0.0142(2) 0.00783(18) 0.00095(16) 0.00083(14) 0.00005(14)
V4 0.00886(18) 0.0136(2) 0.00747(18) -0.00038(16) 0.00089(14) -0.00028(14)
F8 0.0131(6) 0.0279(9) 0.0073(6) 0.0001(6) 0.0003(5) 0.0005(6)
F10 0.0149(7) 0.0174(8) 0.0079(6) 0.0007(6) 0.0014(5) -0.0010(5)
F5 0.0133(6) 0.0241(9) 0.0074(6) 0.0003(6) 0.0010(5) 0.0008(6)
F9 0.0143(7) 0.0175(8) 0.0075(6) -0.0008(6) 0.0012(5) 0.0010(5)
O3 0.0171(9) 0.0166(10) 0.0181(9) 0.0018(8) 0.0005(7) 0.0023(7)
O2 0.0182(9) 0.0171(10) 0.0196(9) 0.0018(8) 0.0028(7) -0.0010(7)
O1 0.0169(9) 0.0175(10) 0.0199(9) -0.0007(8) 0.0019(7) 0.0003(7)
O4 0.0168(9) 0.0189(10) 0.0175(9) -0.0028(8) 0.0011(7) -0.0010(7)
F4 0.0093(6) 0.0205(8) 0.0112(6) -0.0006(6) 0.0010(5) -0.0001(6)
F2 0.0156(7) 0.0166(8) 0.0071(6) 0.0005(6) -0.0003(5) 0.0011(5)
F6 0.0095(6) 0.0229(8) 0.0120(6) 0.0012(6) 0.0002(5) 0.0005(5)
F3 0.0143(7) 0.0160(8) 0.0091(6) 0.0012(6) 0.0002(5) 0.0017(5)
F7 0.0101(6) 0.0219(8) 0.0121(6) -0.0004(6) 0.0000(5) -0.0001(5)
F1 0.0104(6) 0.0214(8) 0.0128(6) 0.0003(6) 0.0013(5) 0.0003(5)
N1 0.0186(11) 0.0233(14) 0.0216(12) -0.0086(11) 0.0018(9) 0.0009(9)
N2 0.0253(13) 0.0296(16) 0.0342(15) 0.0133(12) 0.0007(11) -0.0051(11)
C5 0.0203(13) 0.0214(15) 0.0277(15) 0.0040(12) -0.0019(11) 0.0001(11)
C7 0.0254(14) 0.0284(18) 0.0245(14) -0.0015(12) 0.0062(12) 0.0050(12)
C6 0.0225(13) 0.0164(14) 0.0363(17) -0.0051(13) -0.0031(12) -0.0022(10)
C4 0.0262(14) 0.0343(18) 0.0158(12) 0.0015(12) 0.0055(11) -0.0001(12)
C2 0.0291(16) 0.0175(15) 0.0309(15) 0.0051(12) -0.0018(13) 0.0028(11)
C3 0.0208(13) 0.0265(17) 0.0303(15) -0.0108(13) 0.0050(11) 0.0027(11)
C8 0.0210(13) 0.0217(16) 0.0364(17) 0.0078(13) 0.0066(12) -0.0023(11)
C9 0.0278(15) 0.0221(16) 0.0340(16) -0.0059(13) -0.0042(13) 0.0027(11)
C1 0.0238(13) 0.0344(18) 0.0145(12) 0.0016(12) 0.0015(10) -0.0020(12)
C10 0.0327(16) 0.038(2) 0.0209(14) 0.0017(14) 0.0043(12) 0.0055(14)

_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 1.588(2) . ?
V1 F2 1.9434(14) . ?
V1 F5 1.9544(14) . ?
V1 F1 1.9588(13) . ?
V1 F4 1.9729(14) . ?
V1 F3 2.1762(15) . ?
V2 O2 1.592(2) . ?
V2 F8 1.9501(14) . ?
V2 F6 1.9589(14) . ?
V2 F7 1.9623(14) . ?
V2 F3 1.9655(14) 4_665 ?
V2 F2 2.1253(15) 4_665 ?
V3 O3 1.5990(19) . ?
V3 F5 1.9439(14) . ?
V3 F7 1.9552(14) 1_455 ?
V3 F6 1.9593(14) . ?
V3 F9 1.9769(14) . ?
V3 F10 2.1288(15) 4_565 ?
V4 O4 1.589(2) . ?
V4 F10 1.9409(14) . ?
V4 F8 1.9510(14) . ?
V4 F1 1.9560(14) 1_655 ?
V4 F4 1.9770(14) . ?
V4 F9 2.1930(15) 4_666 ?
F10 V3 2.1288(15) 4_666 ?
F9 V4 2.1930(15) 4_565 ?
F2 V2 2.1253(15) 4_566 ?
F3 V2 1.9655(14) 4_566 ?
F7 V3 1.9552(14) 1_655 ?
F1 V4 1.9560(14) 1_455 ?
N1 C5 1.342(4) . ?
N1 C1 1.343(4) . ?
N1 H11 0.90(4) . ?
N2 C10 1.330(4) . ?
N2 C6 1.358(4) . ?
N2 H21 0.97(4) . ?
C5 C4 1.378(4) . ?
C5 H5 0.9500 . ?
C7 C6 1.364(4) . ?
C7 C8 1.373(4) . ?
C7 H7 0.9500 . ?
C6 H6 0.9500 . ?
C4 C3 1.380(4) . ?
C4 H4 0.9500 . ?
C2 C1 1.372(4) . ?
C2 C3 1.393(4) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C8 C9 1.388(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(5) . ?
C9 H9 0.9500 . ?
C1 H1 0.9500 . ?

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 F2 99.42(8) . . ?
O1 V1 F5 102.09(8) . . ?
F2 V1 F5 158.48(7) . . ?
O1 V1 F1 97.05(8) . . ?
F2 V1 F1 87.69(6) . . ?
F5 V1 F1 89.31(6) . . ?
O1 V1 F4 99.12(8) . . ?
F2 V1 F4 90.92(6) . . ?
F5 V1 F4 86.07(6) . . ?
F1 V1 F4 163.78(7) . . ?
O1 V1 F3 172.84(8) . . ?
F2 V1 F3 73.42(6) . . ?
F5 V1 F3 85.06(6) . . ?
F1 V1 F3 82.65(6) . . ?
F4 V1 F3 81.47(6) . . ?
O2 V2 F8 103.94(8) . . ?
O2 V2 F6 98.04(8) . . ?
F8 V2 F6 86.42(6) . . ?
O2 V2 F7 95.27(8) . . ?
F8 V2 F7 90.64(6) . . ?
F6 V2 F7 166.69(7) . . ?
O2 V2 F3 98.62(8) . 4_665 ?
F8 V2 F3 157.43(7) . 4_665 ?
F6 V2 F3 91.32(6) . 4_665 ?
F7 V2 F3 86.42(6) . 4_665 ?
O2 V2 F2 172.62(8) . 4_665 ?
F8 V2 F2 83.27(6) . 4_665 ?
F6 V2 F2 83.85(6) . 4_665 ?
F7 V2 F2 82.91(6) . 4_665 ?
F3 V2 F2 74.16(6) 4_665 4_665 ?
O3 V3 F5 104.26(8) . . ?
O3 V3 F7 96.76(8) . 1_455 ?
F5 V3 F7 88.11(6) . 1_455 ?
O3 V3 F6 97.17(8) . . ?
F5 V3 F6 89.07(6) . . ?
F7 V3 F6 166.06(7) 1_455 . ?
O3 V3 F9 97.28(8) . . ?
F5 V3 F9 158.45(7) . . ?
F7 V3 F9 89.05(6) 1_455 . ?
F6 V3 F9 88.57(6) . . ?
O3 V3 F10 171.36(8) . 4_565 ?
F5 V3 F10 84.33(6) . 4_565 ?
F7 V3 F10 84.27(6) 1_455 4_565 ?
F6 V3 F10 81.86(6) . 4_565 ?
F9 V3 F10 74.13(6) . 4_565 ?
O4 V4 F10 100.25(8) . . ?
O4 V4 F8 102.12(8) . . ?
F10 V4 F8 157.60(7) . . ?
O4 V4 F1 97.90(8) . 1_655 ?
F10 V4 F1 88.86(6) . 1_655 ?
F8 V4 F1 86.89(6) . 1_655 ?
O4 V4 F4 97.80(8) . . ?
F10 V4 F4 89.09(6) . . ?
F8 V4 F4 89.09(6) . . ?
F1 V4 F4 164.28(7) 1_655 . ?
O4 V4 F9 173.51(7) . 4_666 ?
F10 V4 F9 73.36(6) . 4_666 ?
F8 V4 F9 84.30(6) . 4_666 ?
F1 V4 F9 83.32(6) 1_655 4_666 ?
F4 V4 F9 81.16(6) . 4_666 ?
V2 F8 V4 144.78(9) . . ?
V4 F10 V3 108.12(7) . 4_666 ?
V3 F5 V1 145.97(9) . . ?
V3 F9 V4 104.37(6) . 4_565 ?
V1 F4 V4 139.02(8) . . ?
V1 F2 V2 107.58(7) . 4_566 ?
V2 F6 V3 142.48(9) . . ?
V2 F3 V1 104.84(6) 4_566 . ?
V3 F7 V2 160.18(8) 1_655 . ?
V4 F1 V1 162.49(8) 1_455 . ?
C5 N1 C1 123.0(3) . . ?
C5 N1 H11 117(3) . . ?
C1 N1 H11 120(3) . . ?
C10 N2 C6 122.2(3) . . ?
C10 N2 H21 125(3) . . ?
C6 N2 H21 112(3) . . ?
N1 C5 C4 119.2(3) . . ?
N1 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C6 C7 C8 119.8(3) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
N2 C6 C7 119.1(3) . . ?
N2 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C1 C2 C3 118.7(3) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 120.3(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C7 C8 C9 120.2(3) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 118.4(3) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N1 C1 C2 119.7(3) . . ?
N1 C1 H1 120.2 . . ?
C2 C1 H1 120.2 . . ?
N2 C10 C9 120.4(3) . . ?
N2 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?

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
N2 H21 F3 0.97(4) 1.95(4) 2.791(3) 144(4) .
N2 H21 F4 0.97(4) 2.28(5) 3.060(3) 137(3) .
N2 H21 F7 0.97(4) 2.59(4) 3.123(3) 115(3) 4_566
N1 H11 F9 0.90(4) 1.78(4) 2.667(3) 169(4) .

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        33.57
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.098