
 
#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------#
 
data_global

#------------------ AUTHOR DETAILS -------------------------------------------#

# Name and address of author for correspondence

_publ_contact_author_name        'Le Fur, Eric'
_publ_contact_author_address     
;ENSCR
;
_publ_contact_author_email       eric.le-fur@ensc-rennes.fr
_publ_contact_author_fax         00(000)0000000
loop_
_publ_author_name
_publ_author_address
'Gautier, Romain'
;
;
'Le Fur, Eric'
;
;

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date             2013-11-22
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#
 
data_import

_audit_creation_date             2013-11-22T06:30:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category         FI

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        ?
_chemical_formula_moiety         'O9 P V2, 2(O), K'
_chemical_formula_sum            'K O11 P V2'
_chemical_compound_source        'synthesis as described'
_chemical_formula_weight         347.95

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19
_chemical_absolute_configuration unk
_symmetry_space_group_name_Hall  'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   7.12030(10)
_cell_length_b                   10.1782(2)
_cell_length_c                   12.3477(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     894.86(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9473
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      32.032
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_diffrn_ambient_temperature      293(2)
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_diffrn    2.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -8 0.043
0 1 8 0.033
1 0 0 0.135
-1 0 0 0.176
0 1 0 0.036
0 -1 0 0.015
0 0 1 0.026
0 0 -1 0.03

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.779
_exptl_absorpt_correction_type   none
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.100616
_diffrn_orient_matrix_ub_12      -0.464573E-1
_diffrn_orient_matrix_ub_13      0.415458E-1
_diffrn_orient_matrix_ub_21      0.539388E-1
_diffrn_orient_matrix_ub_22      -0.865715E-1
_diffrn_orient_matrix_ub_23      -0.223392E-1
_diffrn_orient_matrix_ub_31      0.818015E-1
_diffrn_orient_matrix_ub_32      -0.582E-4
_diffrn_orient_matrix_ub_33      0.658313E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_number            15601
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.86
_diffrn_reflns_theta_max         32
_diffrn_reflns_theta_full        32
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             3096
_reflns_number_gt                2950
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0205P)²+1.4939P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3096
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0687
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_restrained_S_all      1.217
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.112

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.006 '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'
K K 0.2009 0.2494 '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'

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 0.19714(6) -0.03709(4) 0.09371(4) 0.00844(9) Uani 1 1 d . . .
V2 V 0.01919(5) 0.27777(4) -0.00432(4) 0.00727(8) Uani 1 1 d . . .
K1 K 0.25168(10) 0.26596(7) 0.26327(6) 0.02321(14) Uani 1 1 d . . .
P1 P 0.23596(9) 0.07231(6) -0.14391(5) 0.00715(11) Uani 1 1 d . . .
O7 O -0.0840(3) 0.34431(19) 0.13151(16) 0.0097(3) Uani 1 1 d . . .
O2 O 0.4467(3) 0.09702(19) 0.07810(16) 0.0107(3) Uani 1 1 d . . .
O1 O 0.0583(3) -0.1597(2) 0.11130(18) 0.0152(4) Uani 1 1 d . . .
O9 O 0.2440(3) 0.31080(17) 0.01684(16) 0.0106(3) Uani 1 1 d . . .
O8 O 0.0623(3) 0.15973(19) -0.12596(15) 0.0097(3) Uani 1 1 d . . .
O4 O 0.2740(3) -0.0110(2) 0.24350(15) 0.0114(4) Uani 1 1 d . . .
OW1 O 0.2524(4) 0.5377(3) 0.2699(2) 0.0277(5) Uani 1 1 d . . .
O3 O 0.4413(3) -0.1729(2) 0.08453(19) 0.0153(4) Uani 1 1 d . . .
OW2 O 0.2467(4) 0.5960(2) 0.0485(2) 0.0245(5) Uani 1 1 d . . .
O5 O 0.2352(3) -0.04370(19) -0.06340(14) 0.0108(3) Uani 1 1 d . . .
O6 O 0.0531(3) 0.09414(19) 0.08831(17) 0.0115(3) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 1.606(2) . ?
V1 O6 1.685(2) . ?
V1 O4 1.9471(19) . ?
V1 O5 1.9599(18) . ?
V1 O3 2.224(2) . ?
V1 O2 2.2491(19) . ?
V1 K1 3.7481(9) . ?
V2 O2 1.6493(19) 3_455 ?
V2 O9 1.6563(19) . ?
V2 O8 1.9477(19) . ?
V2 O7 1.9525(19) . ?
V2 O9 2.1625(19) 3_455 ?
V2 O6 2.205(2) . ?
V2 K1 3.6976(9) . ?
V2 K1 3.7483(8) 3_455 ?
K1 OW1 2.767(3) . ?
K1 O1 2.801(2) 4 ?
K1 O4 2.834(2) . ?
K1 O8 2.888(2) 3 ?
K1 O3 2.949(2) 4_655 ?
K1 O7 3.000(2) . ?
K1 O9 3.077(2) . ?
K1 O5 3.116(2) 2 ?
K1 O6 3.118(2) . ?
K1 O2 3.180(2) . ?
K1 P1 3.6298(10) 2 ?
P1 O4 1.526(2) 2_554 ?
P1 O8 1.5392(19) . ?
P1 O5 1.5436(19) . ?
P1 O7 1.5447(19) 3 ?
P1 K1 3.6298(10) 2_554 ?
O7 P1 1.5447(19) 3_455 ?
O2 V2 1.6493(19) 3 ?
O1 K1 2.801(2) 4_545 ?
O9 V2 2.1625(19) 3 ?
O8 K1 2.888(2) 3_455 ?
O4 P1 1.526(2) 2 ?
O3 K1 2.949(2) 4_645 ?
O5 K1 3.116(2) 2_554 ?

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 O6 104.26(10) . . ?
O1 V1 O4 98.66(10) . . ?
O6 V1 O4 95.76(9) . . ?
O1 V1 O5 101.09(10) . . ?
O6 V1 O5 94.15(10) . . ?
O4 V1 O5 154.96(9) . . ?
O1 V1 O3 90.31(9) . . ?
O6 V1 O3 165.08(9) . . ?
O4 V1 O3 85.04(8) . . ?
O5 V1 O3 79.63(8) . . ?
O1 V1 O2 165.72(9) . . ?
O6 V1 O2 89.80(8) . . ?
O4 V1 O2 77.08(8) . . ?
O5 V1 O2 80.02(8) . . ?
O3 V1 O2 75.82(7) . . ?
O1 V1 K1 128.85(8) . . ?
O6 V1 K1 55.45(7) . . ?
O4 V1 K1 47.77(6) . . ?
O5 V1 K1 124.53(6) . . ?
O3 V1 K1 117.31(6) . . ?
O2 V1 K1 57.76(5) . . ?
O2 V2 O9 103.45(9) 3_455 . ?
O2 V2 O8 95.74(9) 3_455 . ?
O9 V2 O8 95.42(9) . . ?
O2 V2 O7 95.08(9) 3_455 . ?
O9 V2 O7 99.08(9) . . ?
O8 V2 O7 159.35(9) . . ?
O2 V2 O9 89.95(8) 3_455 3_455 ?
O9 V2 O9 166.31(4) . 3_455 ?
O8 V2 O9 80.25(8) . 3_455 ?
O7 V2 O9 82.23(8) . 3_455 ?
O2 V2 O6 167.41(9) 3_455 . ?
O9 V2 O6 89.11(8) . . ?
O8 V2 O6 81.94(8) . . ?
O7 V2 O6 83.66(8) . . ?
O9 V2 O6 77.46(7) 3_455 . ?
O2 V2 K1 131.20(7) 3_455 . ?
O9 V2 K1 55.46(7) . . ?
O8 V2 K1 126.75(6) . . ?
O7 V2 K1 54.00(6) . . ?
O9 V2 K1 117.13(5) 3_455 . ?
O6 V2 K1 57.30(5) . . ?
O2 V2 K1 57.43(7) 3_455 3_455 ?
O9 V2 K1 130.53(7) . 3_455 ?
O8 V2 K1 49.39(6) . 3_455 ?
O7 V2 K1 125.64(6) . 3_455 ?
O9 V2 K1 55.18(5) 3_455 3_455 ?
O6 V2 K1 113.43(6) . 3_455 ?
K1 V2 K1 170.370(15) . 3_455 ?
OW1 K1 O1 73.44(7) . 4 ?
OW1 K1 O4 175.34(7) . . ?
O1 K1 O4 111.15(6) 4 . ?
OW1 K1 O8 75.77(7) . 3 ?
O1 K1 O8 149.04(6) 4 3 ?
O4 K1 O8 99.61(6) . 3 ?
OW1 K1 O3 76.63(7) . 4_655 ?
O1 K1 O3 100.06(6) 4 4_655 ?
O4 K1 O3 102.90(6) . 4_655 ?
O8 K1 O3 75.59(6) 3 4_655 ?
OW1 K1 O7 75.63(7) . . ?
O1 K1 O7 66.42(6) 4 . ?
O4 K1 O7 105.22(6) . . ?
O8 K1 O7 102.85(6) 3 . ?
O3 K1 O7 151.67(6) 4_655 . ?
OW1 K1 O9 83.16(7) . . ?
O1 K1 O9 119.52(6) 4 . ?
O4 K1 O9 93.63(5) . . ?
O8 K1 O9 52.72(5) 3 . ?
O3 K1 O9 127.73(6) 4_655 . ?
O7 K1 O9 53.85(5) . . ?
OW1 K1 O5 134.86(7) . 2 ?
O1 K1 O5 80.79(6) 4 2 ?
O4 K1 O5 48.34(5) . 2 ?
O8 K1 O5 124.79(6) 3 2 ?
O3 K1 O5 72.14(6) 4_655 2 ?
O7 K1 O5 126.12(6) . 2 ?
O9 K1 O5 141.95(5) . 2 ?
OW1 K1 O6 125.58(7) . . ?
O1 K1 O6 100.22(6) 4 . ?
O4 K1 O6 53.70(6) . . ?
O8 K1 O6 95.02(6) 3 . ?
O3 K1 O6 153.62(6) 4_655 . ?
O7 K1 O6 53.98(5) . . ?
O9 K1 O6 52.42(5) . . ?
O5 K1 O6 94.72(5) 2 . ?
OW1 K1 O2 124.12(7) . . ?
O1 K1 O2 152.61(6) 4 . ?
O4 K1 O2 51.37(5) . . ?
O8 K1 O2 52.05(5) 3 . ?
O3 K1 O2 104.40(6) 4_655 . ?
O7 K1 O2 95.84(5) . . ?
O9 K1 O2 51.47(5) . . ?
O5 K1 O2 95.06(5) 2 . ?
O6 K1 O2 52.89(5) . . ?
OW1 K1 P1 159.84(6) . 2 ?
O1 K1 P1 95.79(5) 4 2 ?
O4 K1 P1 23.42(4) . 2 ?
O8 K1 P1 114.53(4) 3 2 ?
O3 K1 P1 88.91(4) 4_655 2 ?
O7 K1 P1 116.28(4) . 2 ?
O9 K1 P1 116.96(4) . 2 ?
O5 K1 P1 24.99(4) 2 2 ?
O6 K1 P1 72.41(4) . 2 ?
O2 K1 P1 72.76(4) . 2 ?
OW1 K1 V2 89.70(6) . . ?
O1 K1 V2 97.62(5) 4 . ?
O4 K1 V2 88.88(4) . . ?
O8 K1 V2 79.03(4) 3 . ?
O3 K1 V2 153.43(5) 4_655 . ?
O7 K1 V2 31.78(4) . . ?
O9 K1 V2 26.32(4) . . ?
O5 K1 V2 130.61(4) 2 . ?
O6 K1 V2 36.50(4) . . ?
O2 K1 V2 64.57(4) . . ?
P1 K1 V2 108.90(2) 2 . ?
O4 P1 O8 109.29(11) 2_554 . ?
O4 P1 O5 105.88(11) 2_554 . ?
O8 P1 O5 110.29(11) . . ?
O4 P1 O7 110.72(12) 2_554 3 ?
O8 P1 O7 109.54(10) . 3 ?
O5 P1 O7 111.06(11) . 3 ?
O4 P1 K1 47.57(8) 2_554 2_554 ?
O8 P1 K1 127.83(8) . 2_554 ?
O5 P1 K1 58.52(7) . 2_554 ?
O7 P1 K1 122.16(8) 3 2_554 ?
P1 O7 V2 126.02(12) 3_455 . ?
P1 O7 K1 138.90(11) 3_455 . ?
V2 O7 K1 94.22(7) . . ?
V2 O2 V1 139.77(11) 3 . ?
V2 O2 K1 96.66(8) 3 . ?
V1 O2 K1 85.50(6) . . ?
V1 O1 K1 140.32(11) . 4_545 ?
V2 O9 V2 141.24(10) . 3 ?
V2 O9 K1 98.23(8) . . ?
V2 O9 K1 89.58(6) 3 . ?
P1 O8 V2 126.47(11) . . ?
P1 O8 K1 133.00(10) . 3_455 ?
V2 O8 K1 99.81(7) . 3_455 ?
P1 O4 V1 142.81(14) 2 . ?
P1 O4 K1 109.02(10) 2 . ?
V1 O4 K1 101.65(8) . . ?
V1 O3 K1 132.70(9) . 4_645 ?
P1 O5 V1 127.71(12) . . ?
P1 O5 K1 96.48(8) . 2_554 ?
V1 O5 K1 135.16(9) . 2_554 ?
V1 O6 V2 139.38(11) . . ?
V1 O6 K1 98.11(8) . . ?
V2 O6 K1 86.20(6) . . ?

# END of CIF
