# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_1
_database_code_depnum_ccdc_archive 'CCDC 1486615'
_audit_update_record             
;
2017-01-16 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-15
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(O102 P12 V30), 8(H0.5 O0.25), 1(O), 12(H3 N0.75)'
_chemical_formula_sum            'H42 N9 O54 P6 V15'
_chemical_formula_weight         1982.34
_chemical_melting_point          ?
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'
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'
P P 0.1023 0.0942 '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      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'y, x, -z'
'-x, y, -z'
'-y, -x, -z'
'z, x, y'
'-x, z, y'
'-z, -x, y'
'x, -z, y'
'z, -x, -y'
'x, z, -y'
'-z, x, -y'
'-x, -z, -y'
'y, z, x'
'-z, -y, -x'
'-z, y, x'
'z, y, -x'
'z, -y, x'
'y, -z, -x'
'-y, -z, x'
'-y, z, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'x+1/2, z+1/2, -y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z'
'-y, -x, z'
'x, -y, z'
'y, x, z'
'-z, -x, -y'
'x, -z, -y'
'z, x, -y'
'-x, z, -y'
'-z, x, y'
'-x, -z, y'
'z, -x, y'
'x, z, y'
'-y, -z, -x'
'z, y, x'
'z, -y, -x'
'-z, -y, x'
'-z, y, -x'
'-y, z, x'
'y, z, -x'
'y, -z, x'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, x+1/2, -y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'z+1/2, -x+1/2, y+1/2'
'x+1/2, z+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'

_cell_length_a                   16.0271(5)
_cell_length_b                   16.0271(5)
_cell_length_c                   16.0271(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4116.8(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3554
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.442
_cell_measurement_theta_min      2.542
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.818
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13392
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.442
_diffrn_reflns_theta_min         5.398
_diffrn_ambient_temperature      298.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                457
_reflns_number_total             495
_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 v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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         1.408
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         495
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0842
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1469P)²+43.9141P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2524
_refine_ls_wR_factor_ref         0.2560
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H,H) groups, All O(H) groups
2. Restrained distances
 V2-O2
 2 with sigma of 0.02
 V1-O2
 2 with sigma of 0.02
 O3-V2
 1.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: V1(0.0625) V2(0.25) O1(0.0625) O2(0.25) O3(0.25) O1W(0.04167)
 H1W(0.08334) O2W(0.02083) N1(0.1875) H1A(0.1875) H1B(0.1875) H1C(0.375)
 Fixed X: O1W(0.25)
 Fixed Y: O1W(0.75)
 Fixed Z: O1W(0.75)
5.a Riding coordinates:
 O1W(H1W), N1(H1A,H1B,H1C)
;
_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
V1 V 0.3224(3) 1.0000 1.0000 0.0224(10) Uani 0.5 8 d DS T P . .
V2 V 0.40937(14) 0.88551(10) 0.88551(10) 0.0248(8) Uani 0.5 2 d DS T P A .
P1 P 0.5000 1.0000 0.7500 0.0243(9) Uani 1 8 d S T P . .
O1 O 0.2220(14) 1.0000 1.0000 0.047(6) Uani 0.5 8 d S T P A .
O2 O 0.3669(6) 0.8881(6) 1.0030(14) 0.023(2) Uani 0.25 1 d D . . A -1
O3 O 0.3404(7) 0.828(2) 0.842(2) 0.028(7) Uani 0.25 1 d D U . A -1
O4 O 0.5000 0.9216(3) 0.8046(3) 0.0305(12) Uani 1 2 d S T P A 1
O1W O 0.2500 0.7500 0.7500 0.27(2) Uani 0.5 12 d S TU P . .
H1W H 0.2765 0.7796 0.7796 0.401 Uiso 0.1667 2 d RS T P . .
O2W O 0.359(7) 0.641(7) 0.641(7) 0.13(2) Uani 0.125 6 d S TU P . .
N1 N 0.5000 0.7406(10) 0.7406(10) 0.091(7) Uani 0.75 4 d S T P . .
H1A H 0.5000 0.7024 0.7734 0.136 Uiso 0.375 2 d RS T P . .
H1B H 0.5000 0.7894 0.7645 0.136 Uiso 0.375 2 d RS T P . .
H1C H 0.4528 0.7418 0.7085 0.136 Uiso 0.375 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 0.0181(19) 0.0246(13) 0.0246(13) 0.000 0.000 0.000
V2 0.0303(13) 0.0220(9) 0.0220(9) -0.0007(8) -0.0010(6) -0.0010(6)
P1 0.0280(12) 0.0280(12) 0.0168(15) 0.000 0.000 0.000
O1 0.022(10) 0.059(9) 0.059(9) 0.000 0.000 0.000
O2 0.026(5) 0.026(4) 0.018(5) -0.001(16) -0.013(15) -0.003(4)
O3 0.031(5) 0.025(12) 0.026(12) 0.013(11) -0.007(5) -0.013(5)
O4 0.039(3) 0.027(2) 0.025(2) 0.0043(18) 0.000 0.000
O1W 0.27(2) 0.27(2) 0.27(2) -0.001(12) 0.001(12) 0.001(12)
O2W 0.13(2) 0.13(2) 0.13(2) 0.001(12) -0.001(12) -0.001(12)
N1 0.15(2) 0.060(8) 0.060(8) 0.023(9) 0.000 0.000

_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 V2 2.945(3) 5_577 ?
V1 V2 2.945(3) 55_575 ?
V1 V2 2.945(3) 51_557 ?
V1 V2 2.945(3) . ?
V1 O1 1.61(2) . ?
V1 O2 1.931(9) . ?
V2 V2 2.905(5) 53_655 ?
V2 O2 2.00(2) . ?
V2 O3 1.600(11) . ?
V2 O4 2.031(4) . ?
V2 O4 2.031(4) 10_655 ?
P1 O4 1.532(5) . ?
P1 O4 1.532(5) 76_656 ?
P1 O4 1.532(5) 3_675 ?
P1 O4 1.532(5) 74_466 ?
O4 V2 2.031(4) 53_655 ?
O1W H1W 0.7930 . ?
N1 H1A 0.8074 . ?
N1 H1B 0.8705 . ?
N1 H1C 0.9154 . ?

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
V2 V1 V2 77.07(7) 5_577 55_575 ?
V2 V1 V2 77.07(7) 5_577 51_557 ?
V2 V1 V2 77.07(7) 51_557 . ?
V2 V1 V2 77.07(7) 55_575 . ?
V2 V1 V2 123.54(17) 5_577 . ?
V2 V1 V2 123.54(17) 55_575 51_557 ?
O1 V1 V2 118.23(8) . 51_557 ?
O1 V1 V2 118.23(8) . 55_575 ?
O1 V1 V2 118.23(8) . . ?
O1 V1 V2 118.23(8) . 5_577 ?
O1 V1 O2 111.6(3) . . ?
O2 V1 V2 112.9(5) . 5_577 ?
O2 V1 V2 39.7(6) . 51_557 ?
O2 V1 V2 114.8(5) . 55_575 ?
O2 V1 V2 42.5(6) . . ?
V2 V2 V1 118.23(9) 53_655 . ?
O2 V2 V1 40.6(3) . . ?
O2 V2 V2 109.9(4) . 53_655 ?
O2 V2 O4 89.4(3) . 10_655 ?
O2 V2 O4 146.9(4) . . ?
O3 V2 V1 107.7(5) . . ?
O3 V2 V2 133.7(5) . 53_655 ?
O3 V2 O2 100.8(13) . . ?
O3 V2 O4 104.5(12) . 10_655 ?
O3 V2 O4 112.3(12) . . ?
O4 V2 V1 123.96(16) 10_655 . ?
O4 V2 V1 123.96(16) . . ?
O4 V2 V2 44.34(11) 10_655 53_655 ?
O4 V2 V2 44.34(11) . 53_655 ?
O4 V2 O4 81.5(2) 10_655 . ?
O4 P1 O4 110.3(4) . 3_675 ?
O4 P1 O4 109.07(19) . 74_466 ?
O4 P1 O4 110.3(4) 74_466 76_656 ?
O4 P1 O4 109.06(19) 3_675 74_466 ?
O4 P1 O4 109.07(19) . 76_656 ?
O4 P1 O4 109.06(19) 3_675 76_656 ?
V1 O2 V2 96.9(8) . . ?
V2 O4 V2 91.3(2) . 53_655 ?
P1 O4 V2 126.76(18) . 53_655 ?
P1 O4 V2 126.76(18) . . ?
H1A N1 H1B 113.4 . . ?
H1A N1 H1C 112.5 . . ?
H1B N1 H1C 103.2 . . ?

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
O4 P1 O4 V2 63.2(3) 3_675 . . . ?
O4 P1 O4 V2 56.54(18) 76_656 . . 53_655 ?
O4 P1 O4 V2 -56.54(18) 74_466 . . . ?
O4 P1 O4 V2 177.0(4) 74_466 . . 53_655 ?
O4 P1 O4 V2 -177.0(4) 76_656 . . . ?
O4 P1 O4 V2 -63.2(3) 3_675 . . 53_655 ?

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

TITL 1 in Im-3m New: Im-3m
CELL 0.71073 16.0271 16.0271 16.0271 90 90 90
ZERR 2 0.0005 0.0005 0.0005 0 0 0
LATT 2
SYMM -Y,+X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X,+Z
SYMM +X,-Y,-Z
SYMM +Y,+X,-Z
SYMM -X,+Y,-Z
SYMM -Y,-X,-Z
SYMM +Z,+X,+Y
SYMM -X,+Z,+Y
SYMM -Z,-X,+Y
SYMM +X,-Z,+Y
SYMM +Z,-X,-Y
SYMM +X,+Z,-Y
SYMM -Z,+X,-Y
SYMM -X,-Z,-Y
SYMM +Y,+Z,+X
SYMM -Z,-Y,-X
SYMM -Z,+Y,+X
SYMM +Z,+Y,-X
SYMM +Z,-Y,+X
SYMM +Y,-Z,-X
SYMM -Y,-Z,+X
SYMM -Y,+Z,-X
SFAC H N O P V
UNIT 84 18 108 12 30
DFIX 2 V2 O2
DFIX 2 V1 O2
DFIX 1.6 O3 V2
ISOR 0.01 0.02 O3
ISOR 0.01 0.02 O2W
ISOR 0.01 0.02 O1W

L.S. 20 0 1
PLAN  5
TEMP 24.85
FREE O3 H1W
BOND $H
MORE -1
CONF
fmap 2
acta
SHEL 4 0.77
REM <olex2.extras>
REM <HklSrc "%.\\1.hkl">
REM </olex2.extras>

WGHT    0.146900   43.914101
FVAR       0.05408
V1    5    0.322443    1.000000    1.000000    10.06250    0.01811    0.02462 =
         0.02462    0.00000    0.00000    0.00000
V2    5    0.409372    0.885512    0.885512    10.25000    0.03032    0.02203 =
         0.02203   -0.00070   -0.00099   -0.00099
P1    4    0.500000    1.000000    0.750000    10.12500    0.02805    0.02805 =
         0.01682    0.00000    0.00000    0.00000
O1    3    0.221993    1.000000    1.000000    10.06250    0.02233    0.05900 =
         0.05900    0.00000    0.00000    0.00000
PART -1
O2    3    0.366874    0.888083    1.003035    10.25000    0.02613    0.02622 =
         0.01788   -0.00093   -0.01302   -0.00319
O3    3    0.340418    0.827951    0.842004    10.25000    0.03142    0.02539 =
         0.02577    0.01304   -0.00715   -0.01271
PART 0
PART 1
O4    3    0.500000    0.921583    0.804618    10.50000    0.03935    0.02738 =
         0.02487    0.00425    0.00000    0.00000

PART 0
O1W   3   10.250000   10.750000   10.750000    10.04167    0.26742    0.26742 =
         0.26742   -0.00146    0.00146    0.00146
AFIX   3
H1W   1    0.276490    0.779550    0.779550    10.08334   -1.50000
AFIX   0

O2W   3    0.358649    0.641351    0.641351    10.02083    0.13162    0.13162 =
         0.13162    0.00078   -0.00078   -0.00078
N1    2    0.500000    0.740626    0.740626    10.18750    0.15151    0.06020 =
         0.06020    0.02276    0.00000    0.00000
AFIX   3
H1A   1    0.500000    0.702375    0.773410    10.18750   -1.50000
H1B   1    0.500000    0.789425    0.764470    10.18750   -1.50000
H1C   1    0.452800    0.741806    0.708480    10.37500   -1.50000
AFIX   0
HKLF 4 1 0 1 0 0 0 -1 -1 0 0

REM  1 in Im-3m New: Im-3m
REM R1 =  0.0842 for     457 Fo > 4sig(Fo)  and  0.0881 for all     495 data
REM     48 parameters refined using     21 restraints

END

WGHT      0.1462     43.5666

REM Highest difference peak  1.408,  deepest hole -0.702,  1-sigma level  0.172
Q1    1   0.4521  0.9151  0.9151  10.50000  0.05    1.32
Q2    1   0.5000  1.0000  1.0000  10.06250  0.05    1.20
Q3    1   0.3379  0.8640  0.8640  10.50000  0.05    0.78
Q4    1   0.5000  0.9599  0.7815  10.50000  0.05    0.55
Q5    1   0.3631  0.8390  0.8390  10.50000  0.05    0.53
;
_shelx_res_checksum              46556
_olex2_submission_special_instructions 'No special instructions were received'

