# 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 2017

####################################################################### 
# 
# 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 1543781'
_audit_update_record             
;
2017-04-13 deposited with the CCDC.
2017-06-01 downloaded from the CCDC.
;
_audit_creation_date             2017-03-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C4 H16 Cd4 N4 O14 V4)'
_chemical_formula_sum            'C2 H8 Cd2 N2 O7 V2'
_chemical_formula_weight         498.78
_chemical_melting_point          ?
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'
Cd Cd -0.8075 1.2024 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.598(5)
_cell_length_b                   5.208(5)
_cell_length_c                   6.304(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     479.3(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2676
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.202
_cell_measurement_theta_min      2.791
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.282
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.456
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       bar
_exptl_crystal_F_000             464
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2230
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.984
_diffrn_reflns_theta_max         24.984
_diffrn_reflns_theta_min         3.520
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                464
_reflns_number_total             464
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.0169(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.295
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         464
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0180
_refine_ls_restrained_S_all      1.280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0245P)²+0.5240P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0476
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Cd1 Cd 0.72866(2) 0.10932(5) 0.5000 0.0123(2) Uani 1 2 d S T P . .
V1 V 0.87842(4) 0.53946(13) 0.5000 0.0080(2) Uani 1 2 d S T P . .
O2 O 0.82963(13) 0.3974(3) 0.2838(3) 0.0149(5) Uani 1 1 d . . . . .
O1 O 0.8521(2) -0.1490(6) 0.5000 0.0171(6) Uani 1 2 d S T P . .
O3 O 1.0000 0.5000 0.5000 0.0188(9) Uani 1 4 d S T P . .
N1 N 0.6275(2) 0.4366(7) 0.5000 0.0131(7) Uani 1 2 d S TU P . .
C1 C 0.5290(3) 0.3789(7) 0.5000 0.0187(10) Uani 1 2 d S TU P . .
H1A H 0.517(3) 0.271(8) 0.372(6) 0.037(10) Uiso 1 1 d . . . . .
H1 H 0.636(3) 0.538(8) 0.393(5) 0.025(9) 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
Cd1 0.0097(3) 0.0117(3) 0.0155(3) 0.000 0.000 0.00099(9)
V1 0.0051(4) 0.0091(4) 0.0097(4) 0.000 0.000 0.0005(2)
O2 0.0165(10) 0.0164(11) 0.0118(10) -0.0003(7) -0.0029(8) -0.0003(7)
O1 0.0127(14) 0.0130(13) 0.0254(17) 0.000 0.000 0.0029(11)
O3 0.010(2) 0.021(2) 0.026(2) 0.000 0.000 0.0013(17)
N1 0.0104(18) 0.0101(16) 0.0187(19) 0.000 0.000 0.0012(13)
C1 0.011(2) 0.014(2) 0.031(3) 0.000 0.000 0.0043(16)

_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
Cd1 V1 3.1301(18) . ?
Cd1 O2 2.506(2) . ?
Cd1 O2 2.268(2) 4_645 ?
Cd1 O2 2.268(2) 7_756 ?
Cd1 O2 2.506(2) 6_556 ?
Cd1 O1 2.249(3) . ?
Cd1 N1 2.255(4) . ?
V1 O2 1.707(2) . ?
V1 O2 1.707(2) 6_556 ?
V1 O1 1.667(3) 1_565 ?
V1 O3 1.7867(9) . ?
O2 Cd1 2.268(2) 7_765 ?
O1 V1 1.667(3) 1_545 ?
O3 V1 1.7868(8) 5_766 ?
N1 C1 1.469(6) . ?
C1 C1 1.520(8) 5_666 ?

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
O2 Cd1 V1 127.62(6) 7_756 . ?
O2 Cd1 V1 127.62(6) 4_645 . ?
O2 Cd1 V1 32.95(5) . . ?
O2 Cd1 V1 32.95(5) 6_556 . ?
O2 Cd1 O2 160.23(8) 4_645 6_556 ?
O2 Cd1 O2 104.16(11) 4_645 7_756 ?
O2 Cd1 O2 94.76(7) 7_756 6_556 ?
O2 Cd1 O2 160.23(8) 7_756 . ?
O2 Cd1 O2 65.89(11) 6_556 . ?
O2 Cd1 O2 94.76(7) 4_645 . ?
O1 Cd1 V1 82.44(10) . . ?
O1 Cd1 O2 90.54(8) . 7_756 ?
O1 Cd1 O2 83.50(9) . 6_556 ?
O1 Cd1 O2 83.50(9) . . ?
O1 Cd1 O2 90.54(8) . 4_645 ?
O1 Cd1 N1 167.64(12) . . ?
N1 Cd1 V1 85.20(11) . . ?
N1 Cd1 O2 86.14(10) . . ?
N1 Cd1 O2 86.14(10) . 6_556 ?
N1 Cd1 O2 97.02(8) . 4_645 ?
N1 Cd1 O2 97.02(8) . 7_756 ?
O2 V1 Cd1 53.00(7) 6_556 . ?
O2 V1 Cd1 53.00(7) . . ?
O2 V1 O2 106.00(15) . 6_556 ?
O2 V1 O3 111.39(7) . . ?
O2 V1 O3 111.39(7) 6_556 . ?
O1 V1 Cd1 122.39(12) 1_565 . ?
O1 V1 O2 109.02(9) 1_565 . ?
O1 V1 O2 109.02(9) 1_565 6_556 ?
O1 V1 O3 109.91(11) 1_565 . ?
O3 V1 Cd1 127.69(5) . . ?
Cd1 O2 Cd1 119.98(9) 7_765 . ?
V1 O2 Cd1 125.14(11) . 7_765 ?
V1 O2 Cd1 94.05(10) . . ?
V1 O1 Cd1 140.05(18) 1_545 . ?
V1 O3 V1 180.0 . 5_766 ?
C1 N1 Cd1 119.1(3) . . ?
N1 C1 C1 112.1(4) . 5_666 ?

_shelx_res_file                  
;
    y.res created by SHELXL-2014/7

TITL y in Pnnm
CELL 0.71069 14.598 5.208 6.304 90 90 90
ZERR 2 0.005 0.005 0.005 0.005 0.005 0.005
LATT 1
SYMM -X,-Y,+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cd N O V
UNIT 4 16 4 4 14 4
ISOR 0.01 0.02 N1 C1

L.S. 10
PLAN  25
LIST 1
fmap 2
ACTA
MERG 2
OMIT -3 50
OMIT 2 0 0
OMIT 6 0 0
OMIT 11 2 5
REM <olex2.extras>
REM <HklSrc "%.\\Y.HKL">
REM </olex2.extras>

WGHT    0.024500    0.524000
EXTI    0.016935
FVAR       0.15969
CD1   3    0.728664    0.109322    0.500000    10.50000    0.00967    0.01167 =
         0.01552    0.00000    0.00000    0.00099
V1    6    0.878416    0.539464    0.500000    10.50000    0.00514    0.00910 =
         0.00973    0.00000    0.00000    0.00046
O2    5    0.829630    0.397372    0.283793    11.00000    0.01651    0.01639 =
         0.01181   -0.00029   -0.00294   -0.00035
O1    5    0.852130   -0.149049    0.500000    10.50000    0.01269    0.01305 =
         0.02542    0.00000    0.00000    0.00286
O3    5    1.000000    0.500000    0.500000    10.25000    0.00968    0.02118 =
         0.02567    0.00000    0.00000    0.00126
N1    4    0.627520    0.436614    0.500000    10.50000    0.01042    0.01013 =
         0.01873    0.00000    0.00000    0.00124
C1    1    0.529049    0.378936    0.500000    10.50000    0.01062    0.01441 =
         0.03099    0.00000    0.00000    0.00430
H1A   2    0.517241    0.270710    0.371663    11.00000    0.03744
H1    2    0.635615    0.538130    0.392637    11.00000    0.02463
HKLF 4

REM  y in Pnnm
REM R1 =  0.0180 for     464 Fo > 4sig(Fo)  and  0.0180 for all     464 data
REM     53 parameters refined using     12 restraints

END

WGHT      0.0245      0.5240

REM Highest difference peak  0.715,  deepest hole -0.553,  1-sigma level  0.167
Q1    1   0.7864  0.0995  0.5000  10.50000  0.05    0.71
Q2    1   0.7324  0.1056  0.3503  11.00000  0.05    0.64
Q3    1   0.6664  0.1068  0.5000  10.50000  0.05    0.62
Q4    1   0.8498  0.4228  0.1912  11.00000  0.05    0.42
Q5    1   0.9403  0.5191  0.5000  10.50000  0.05    0.38
Q6    1   0.5000  0.5000  0.5000  10.25000  0.05    0.38
Q7    1   0.8813  0.3451  0.2749  11.00000  0.05    0.37
Q8    1   0.8223  0.4882  0.3123  11.00000  0.05    0.35
Q9    1   0.5978  0.6561  0.2285  11.00000  0.05    0.31
Q10   1   0.7545  0.5746  0.2859  11.00000  0.05    0.31
Q11   1   0.7631  0.4283  0.2857  11.00000  0.05    0.31
Q12   1   0.8830  0.5064  0.3205  11.00000  0.05    0.29
Q13   1   0.4431  0.0333  0.2817  11.00000  0.05    0.28
Q14   1   0.7682  0.1931  0.2189  11.00000  0.05    0.27
Q15   1   1.0000  0.5000  0.2502  10.50000  0.05    0.27
Q16   1   0.8054 -0.1323  0.5000  10.50000  0.05    0.26
Q17   1   0.6330  0.4246  0.3110  11.00000  0.05    0.25
Q18   1   0.6463  0.2153  0.2960  11.00000  0.05    0.25
Q19   1   0.8910  0.5955  0.2254  11.00000  0.05    0.25
Q20   1   0.6571  0.3044  0.5000  10.50000  0.05    0.25
Q21   1   0.8778  0.6525  0.2396  11.00000  0.05    0.25
Q22   1   0.8382 -0.1571  0.2914  11.00000  0.05    0.23
Q23   1   0.4676  0.2651  0.2655  11.00000  0.05    0.23
Q24   1   0.4738  0.4264  0.2297  11.00000  0.05    0.23
Q25   1   0.7123  0.4985  0.2720  11.00000  0.05    0.21
;
_shelx_res_checksum              86528
_olex2_submission_special_instructions 'No special instructions were received'
