# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_y
_database_code_depnum_ccdc_archive 'CCDC 1506905'
_audit_update_record             
;
2016-12-15 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H4 Ni O8 V2'
_chemical_formula_weight         292.62

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'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   5.536(5)
_cell_length_b                   10.628(5)
_cell_length_c                   11.770(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     692.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4728
_cell_measurement_theta_min      3.46
_cell_measurement_theta_max      28.45

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.807
_exptl_crystal_F_000             568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    5.333
_shelx_estimated_absorpt_T_min   0.339
_shelx_estimated_absorpt_T_max   0.474
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.339
_exptl_absorpt_correction_T_max  0.474
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4728
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.462
_diffrn_reflns_theta_max         28.448
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             921
_reflns_number_gt                897
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0155P)²+2.0516P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0027(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         921
_refine_ls_number_parameters     62
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0205
_refine_ls_wR_factor_ref         0.0475
_refine_ls_wR_factor_gt          0.0471
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.004
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.98056(6) 0.2500 0.04053(3) 0.00630(11) Uani 1 2 d DS T P . .
V1 V 0.80453(6) -0.03166(3) 0.17364(3) 0.00560(10) Uani 1 1 d . . . . .
O1 O 0.8343(3) 0.11975(15) 0.14554(13) 0.0142(3) Uani 1 1 d . . . . .
O1W O 0.6603(4) 0.2500 -0.04906(18) 0.0139(4) Uani 1 2 d DS T P . .
H1W H 0.633(5) 0.1851(8) -0.0897(14) 0.021 Uiso 1 1 d D U . . .
O2 O 0.8839(3) -0.11473(16) 0.06355(13) 0.0162(3) Uani 1 1 d . . . . .
O2W O 1.2946(4) 0.2500 0.1295(2) 0.0224(5) Uani 1 2 d DS T P . .
H2W H 1.372(4) 0.1855(9) 0.108(3) 0.034 Uiso 1 1 d D U . . .
O3 O 0.9966(3) -0.07170(15) 0.29189(13) 0.0131(3) 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
Ni1 0.00793(18) 0.00591(18) 0.00507(17) 0.000 0.00129(12) 0.000
V1 0.00588(16) 0.00545(17) 0.00547(16) -0.00031(11) 0.00097(11) -0.00033(11)
O1 0.0191(7) 0.0091(7) 0.0145(7) 0.0028(6) 0.0035(6) -0.0008(6)
O1W 0.0137(10) 0.0146(10) 0.0133(10) 0.000 -0.0056(8) 0.000
O2 0.0173(8) 0.0163(8) 0.0151(7) -0.0063(6) 0.0045(6) 0.0011(6)
O2W 0.0116(11) 0.0395(16) 0.0161(11) 0.000 -0.0013(9) 0.000
O3 0.0085(7) 0.0180(8) 0.0128(7) 0.0050(6) -0.0023(5) -0.0032(6)

_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
Ni1 O1 2.0246(17) . ?
Ni1 O1 2.0247(17) 8_565 ?
Ni1 O2W 2.029(3) . ?
Ni1 O2 2.0325(17) 5_755 ?
Ni1 O2 2.0325(17) 4_755 ?
Ni1 O1W 2.063(3) . ?
V1 O2 1.6284(16) . ?
V1 O1 1.6511(18) . ?
V1 O3 1.8026(17) . ?
V1 O3 1.803(2) 6_556 ?
O1W H1W 0.852(7) . ?
O2 Ni1 2.0324(17) 5_755 ?
O2W H2W 0.848(7) . ?
O3 V1 1.803(2) 6_656 ?

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 Ni1 O1 86.27(10) . 8_565 ?
O1 Ni1 O2W 91.59(8) . . ?
O1 Ni1 O2W 91.59(8) 8_565 . ?
O1 Ni1 O2 91.83(7) . 5_755 ?
O1 Ni1 O2 177.74(7) 8_565 5_755 ?
O2W Ni1 O2 89.68(8) . 5_755 ?
O1 Ni1 O2 177.74(7) . 4_755 ?
O1 Ni1 O2 91.83(7) 8_565 4_755 ?
O2W Ni1 O2 89.68(8) . 4_755 ?
O2 Ni1 O2 90.04(10) 5_755 4_755 ?
O1 Ni1 O1W 88.19(8) . . ?
O1 Ni1 O1W 88.19(8) 8_565 . ?
O2W Ni1 O1W 179.69(10) . . ?
O2 Ni1 O1W 90.53(7) 5_755 . ?
O2 Ni1 O1W 90.53(7) 4_755 . ?
O2 V1 O1 110.01(8) . . ?
O2 V1 O3 109.10(9) . . ?
O1 V1 O3 109.02(8) . . ?
O2 V1 O3 107.82(8) . 6_556 ?
O1 V1 O3 111.69(8) . 6_556 ?
O3 V1 O3 109.17(6) . 6_556 ?
V1 O1 Ni1 145.96(9) . . ?
Ni1 O1W H1W 115.9(17) . . ?
V1 O2 Ni1 164.32(10) . 5_755 ?
Ni1 O2W H2W 106(2) . . ?
V1 O3 V1 132.51(9) . 6_656 ?

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
O2 V1 O1 Ni1 -15.73(19) . . . . ?
O3 V1 O1 Ni1 103.87(18) . . . . ?
O3 V1 O1 Ni1 -135.41(16) 6_556 . . . ?
O1 V1 O2 Ni1 142.8(4) . . . 5_755 ?
O3 V1 O2 Ni1 23.3(4) . . . 5_755 ?
O3 V1 O2 Ni1 -95.2(4) 6_556 . . 5_755 ?
O2 V1 O3 V1 75.95(15) . . . 6_656 ?
O1 V1 O3 V1 -44.20(15) . . . 6_656 ?
O3 V1 O3 V1 -166.45(8) 6_556 . . 6_656 ?

_refine_diff_density_max         0.652
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.103

_shelx_res_file                  
;

    y.res created by SHELXL-2014/7

TITL Y in Pnma
CELL 0.71069 5.536 10.628 11.77 90 90 90
ZERR 4 0.005 0.005 0.005 0.000 0.000 0.000
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC H  Ni O  V
UNIT 16 4 32 8
MERG 2
OMIT 0 1 1
OMIT 1 4 2
L.S. 40
ACTA
BOND $H
FMAP 2
PLAN 5
LIST 1
EQIV $1 +X,0.5-Y,+Z
DFIX 0.85 0.01 O1W H1W O1W H1W_$1
DFIX 0.85 0.01 O2W H2W O2W H2W_$1
SADI Ni1 H1W Ni1 H1W_$1
SADI Ni1 H2W Ni1 H2W_$1
DANG 1.387 0.02 H1W_$1 H1W
DANG 1.387 0.02 H2W_$1 H2W
MORE -1
CONF
WGHT    0.015500    2.051600
EXTI    0.002725
FVAR       0.15694
NI1   2    0.980561    0.250000    0.040529    10.50000    0.00793    0.00591 =
         0.00507    0.00000    0.00129    0.00000
V1    4    0.804527   -0.031655    0.173641    11.00000    0.00588    0.00545 =
         0.00547   -0.00031    0.00097   -0.00033
O1    3    0.834330    0.119754    0.145539    11.00000    0.01909    0.00908 =
         0.01448    0.00281    0.00346   -0.00075
O1W   3    0.660313    0.250000   -0.049055    10.50000    0.01366    0.01460 =
         0.01331    0.00000   -0.00558    0.00000
H1W   1    0.633498    0.185132   -0.089689    11.00000   -1.50000
O2    3    0.883857   -0.114734    0.063548    11.00000    0.01728    0.01631 =
         0.01513   -0.00632    0.00446    0.00114
O2W   3    1.294623    0.250000    0.129457    10.50000    0.01160    0.03954 =
         0.01612    0.00000   -0.00134    0.00000
H2W   1    1.372084    0.185452    0.107960    11.00000   -1.50000
O3    3    0.996643   -0.071699    0.291891    11.00000    0.00855    0.01799 =
         0.01277    0.00503   -0.00234   -0.00320
HKLF 4

REM  Y in Pnma
REM R1 =  0.0205 for     897 Fo > 4sig(Fo)  and  0.0212 for all     921 data
REM     62 parameters refined using      8 restraints

END

WGHT      0.0155      1.0327

REM Highest difference peak  0.652,  deepest hole -0.688,  1-sigma level  0.103
Q1    1   1.3058  0.2500  0.2024  10.50000  0.05    0.65
Q2    1   1.4282  0.2500  0.0843  10.50000  0.05    0.53
Q3    1   0.8332  0.0351  0.1203  11.00000  0.05    0.36
Q4    1   1.0064  0.2808  0.0957  11.00000  0.05    0.35
Q5    1   0.7413 -0.0828  0.1027  11.00000  0.05    0.35
;
_shelx_res_checksum              53827
