# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Luck, Rudy'
_publ_contact_author_email       rluck@mtu.edu

_publ_section_title              
;
Expanding molecular transition metal cubane clusters of the form
[M4(u3-O)4]12+: Syntheses, spectroscopic and structural
characterizations of molecules M4(u3-O)4(O2P(Bn)2)4(O4) , M = VV and WV+
;
loop_
_publ_author_name
R.Luck
J.Maass
Z.Chen
M.Zeller

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF

# Attachment '- Vanadium.cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2011-06-25 at 13:18:59
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.4
# Request file : c:\wingx\files\archive.reqdat
# CIF files read : 10mz512_0m dreduc sadabs struct

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

data_10mz512_0m
_database_code_depnum_ccdc_archive 'CCDC 834511'
#TrackingRef '- Vanadium.cif'

_audit_creation_date             2011-06-25T13:18:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
Tetrakisdibenzylphosphinato-octaoxo-tetravanadium(V).tetrahydrate
;
_chemical_formula_moiety         'C56 H56 O16 P4 V4, 4(H2 O)'
_chemical_formula_sum            'C56 H64 O20 P4 V4'
_chemical_formula_weight         1384.75
_chemical_compound_source        'synthesis as described'

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

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_Int_Tables_number      88
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   22.306(4)
_cell_length_b                   22.306(4)
_cell_length_c                   12.824(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6380.7(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4266
_cell_measurement_theta_min      2.5827
_cell_measurement_theta_max      30.4582
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2848
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  0.746

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

_diffrn_source                   'sealed x-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'APEX-II CCD'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_ub_11      0.224517E-2
_diffrn_orient_matrix_ub_12      0.446448E-1
_diffrn_orient_matrix_ub_13      -0.5928E-2
_diffrn_orient_matrix_ub_21      -0.195418E-2
_diffrn_orient_matrix_ub_22      -0.331127E-2
_diffrn_orient_matrix_ub_23      -0.776944E-1
_diffrn_orient_matrix_ub_31      -0.44732E-1
_diffrn_orient_matrix_ub_32      0.238545E-2
_diffrn_orient_matrix_ub_33      0.309666E-2
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_number            22239
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_full        28
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_reflns_number_total             4828
_reflns_number_gt                3503
_reflns_threshold_expression     >2\s(I)

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

_computing_data_collection       'Bruker APEX2 software'
_computing_cell_refinement       'SAINT V7.66A integration software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_structure_solution    'SIR-2004 (Altomare et al, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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   geom

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

_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^ > 2\s(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^)+(0.0448P)^2^+5.6540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4828
_refine_ls_number_parameters     211
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.102
_refine_ls_wR_factor_gt          0.0899
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.46
_refine_diff_density_rms         0.074

#----------------------------------------------------------------------------#
# 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
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O10 O 0.0263(4) -0.0300(6) 0.9832(6) 0.079(3) Uani 0.277(4) 1 d P . .
O20 O 0.1602(6) -0.2709(3) 0.7773(6) 0.044(4) Uani 0.201(7) 1 d P . .
O30 O 0.0112(4) -0.1836(6) 0.8872(8) 0.236(8) Uani 0.522(7) 1 d P . .
V1 V -0.030017(14) 0.195879(13) 0.51982(3) 0.01826(9) Uani 1 1 d . . .
O1 O -0.03415(6) 0.18969(6) 0.39740(12) 0.0234(3) Uani 1 1 d . . .
O2 O 0.04627(6) 0.22173(6) 0.54049(11) 0.0195(3) Uani 1 1 d . . .
O3 O -0.11450(6) 0.18088(6) 0.55609(11) 0.0198(3) Uani 1 1 d . . .
O4 O -0.01110(6) 0.11349(6) 0.55626(11) 0.0207(3) Uani 1 1 d . . .
P1 P 0.02739(2) 0.08896(2) 0.64562(4) 0.01845(11) Uani 1 1 d . . .
C1 C -0.02034(9) 0.05926(9) 0.74631(17) 0.0245(4) Uani 1 1 d . . .
H1A H 0.0052 0.0426 0.8024 0.029 Uiso 1 1 calc R . .
H1B H -0.0438 0.0926 0.7767 0.029 Uiso 1 1 calc R . .
C2 C -0.06332(9) 0.01104(9) 0.71069(16) 0.0236(4) Uani 1 1 d . . .
C3 C -0.11831(9) 0.02607(10) 0.66867(18) 0.0276(4) Uani 1 1 d . . .
H3 H -0.1286 0.0671 0.6598 0.033 Uiso 1 1 calc R . .
C4 C -0.15889(10) -0.01815(11) 0.63918(19) 0.0330(5) Uani 1 1 d . . .
H4 H -0.1968 -0.0073 0.6111 0.04 Uiso 1 1 calc R . .
C5 C -0.14398(11) -0.07773(11) 0.65076(19) 0.0351(5) Uani 1 1 d . . .
H5 H -0.172 -0.108 0.6319 0.042 Uiso 1 1 calc R . .
C6 C -0.08853(11) -0.09360(10) 0.6896(2) 0.0346(5) Uani 1 1 d . . .
H6 H -0.0779 -0.1347 0.6952 0.042 Uiso 1 1 calc R . .
C7 C -0.04829(10) -0.04960(9) 0.72043(19) 0.0302(5) Uani 1 1 d . . .
H7 H -0.0104 -0.0607 0.7482 0.036 Uiso 1 1 calc R . .
C8 C 0.07245(8) 0.02957(8) 0.59303(16) 0.0199(4) Uani 1 1 d . . .
H8A H 0.0459 0.0021 0.5537 0.024 Uiso 1 1 calc R . .
H8B H 0.1011 0.0472 0.5426 0.024 Uiso 1 1 calc R . .
C9 C 0.10754(8) -0.00696(8) 0.67133(15) 0.0187(4) Uani 1 1 d . . .
C10 C 0.10558(9) -0.06903(9) 0.66538(17) 0.0246(4) Uani 1 1 d . . .
H10 H 0.0826 -0.0877 0.6121 0.03 Uiso 1 1 calc R . .
C11 C 0.13674(10) -0.10431(10) 0.73618(19) 0.0323(5) Uani 1 1 d . . .
H11 H 0.1352 -0.1468 0.7307 0.039 Uiso 1 1 calc R . .
C12 C 0.16996(10) -0.07790(11) 0.81466(18) 0.0332(5) Uani 1 1 d . . .
H12 H 0.1911 -0.102 0.8634 0.04 Uiso 1 1 calc R . .
C13 C 0.17210(10) -0.01616(11) 0.82173(18) 0.0316(5) Uani 1 1 d . . .
H13 H 0.1947 0.0023 0.8758 0.038 Uiso 1 1 calc R . .
C14 C 0.14148(9) 0.01907(9) 0.75039(17) 0.0253(4) Uani 1 1 d . . .
H14 H 0.1437 0.0615 0.7555 0.03 Uiso 1 1 calc 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
O10 0.083(6) 0.125(9) 0.031(4) 0.043(5) 0.002(4) 0.037(6)
O20 0.100(10) 0.011(4) 0.021(5) 0.000(3) 0.011(5) -0.009(4)
O30 0.096(6) 0.440(18) 0.171(9) 0.183(12) -0.018(5) -0.018(9)
V1 0.01442(15) 0.01498(15) 0.02539(18) -0.00095(12) 0.00000(12) -0.00053(11)
O1 0.0200(7) 0.0214(7) 0.0289(8) -0.0008(6) 0.0001(6) -0.0017(5)
O2 0.0151(6) 0.0150(6) 0.0285(8) 0.0001(5) 0.0010(5) 0.0001(5)
O3 0.0149(6) 0.0160(6) 0.0286(8) -0.0020(5) 0.0015(5) -0.0010(5)
O4 0.0174(6) 0.0152(6) 0.0295(8) -0.0004(5) -0.0019(5) 0.0003(5)
P1 0.0159(2) 0.0142(2) 0.0253(3) -0.00057(18) 0.00123(18) -0.00002(17)
C1 0.0231(9) 0.0224(9) 0.0280(11) -0.0015(8) 0.0045(8) -0.0021(8)
C2 0.0203(9) 0.0225(9) 0.0280(11) -0.0037(8) 0.0099(8) -0.0032(7)
C3 0.0242(10) 0.0263(10) 0.0323(12) -0.0030(9) 0.0043(8) 0.0011(8)
C4 0.0232(10) 0.0427(13) 0.0332(13) -0.0051(10) 0.0039(9) -0.0045(9)
C5 0.0374(13) 0.0355(12) 0.0323(13) -0.0084(10) 0.0107(10) -0.0162(10)
C6 0.0414(13) 0.0199(10) 0.0424(14) -0.0015(9) 0.0129(11) -0.0053(9)
C7 0.0247(10) 0.0252(10) 0.0406(13) 0.0032(9) 0.0073(9) -0.0016(8)
C8 0.0181(9) 0.0173(8) 0.0243(10) -0.0015(7) 0.0003(7) 0.0010(7)
C9 0.0160(8) 0.0182(8) 0.0220(10) -0.0010(7) 0.0032(7) 0.0014(7)
C10 0.0222(9) 0.0186(9) 0.0330(12) -0.0034(8) 0.0006(8) -0.0003(7)
C11 0.0321(11) 0.0207(10) 0.0441(14) 0.0074(9) 0.0034(10) 0.0036(9)
C12 0.0306(11) 0.0396(13) 0.0295(12) 0.0109(10) 0.0031(9) 0.0120(10)
C13 0.0297(11) 0.0385(12) 0.0266(11) -0.0067(9) -0.0068(9) 0.0111(9)
C14 0.0247(10) 0.0200(9) 0.0310(12) -0.0073(8) -0.0043(8) 0.0034(8)

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

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
O10 O20 1.345(14) 12_557 ?
O20 O10 1.345(14) 11_657 ?
V1 O1 1.5786(16) . ?
V1 O2 1.8161(13) . ?
V1 O2 1.8919(13) 2 ?
V1 O4 1.9427(13) . ?
V1 O3 1.9697(13) . ?
V1 O2 2.4392(15) 15_556 ?
V1 V1 2.7610(8) 2 ?
O2 V1 1.8919(13) 2 ?
O2 V1 2.4392(15) 16_556 ?
O3 P1 1.5258(14) 15_556 ?
O4 P1 1.5328(14) . ?
P1 O3 1.5258(14) 16_556 ?
P1 C8 1.7944(19) . ?
P1 C1 1.800(2) . ?
C1 C2 1.512(3) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 C3 1.381(3) . ?
C2 C7 1.399(3) . ?
C3 C4 1.391(3) . ?
C3 H3 0.95 . ?
C4 C5 1.378(3) . ?
C4 H4 0.95 . ?
C5 C6 1.380(4) . ?
C5 H5 0.95 . ?
C6 C7 1.388(3) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 C9 1.512(3) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 C10 1.387(3) . ?
C9 C14 1.392(3) . ?
C10 C11 1.388(3) . ?
C10 H10 0.95 . ?
C11 C12 1.382(3) . ?
C11 H11 0.95 . ?
C12 C13 1.381(3) . ?
C12 H12 0.95 . ?
C13 C14 1.386(3) . ?
C13 H13 0.95 . ?
C14 H14 0.95 . ?

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 O2 103.16(7) . . ?
O1 V1 O2 102.31(7) . 2 ?
O2 V1 O2 81.41(6) . 2 ?
O1 V1 O4 99.74(7) . . ?
O2 V1 O4 93.54(6) . . ?
O2 V1 O4 157.95(6) 2 . ?
O1 V1 O3 99.44(7) . . ?
O2 V1 O3 156.33(6) . . ?
O2 V1 O3 87.06(5) 2 . ?
O4 V1 O3 89.44(5) . . ?
O1 V1 O2 177.40(6) . 15_556 ?
O2 V1 O2 79.43(6) . 15_556 ?
O2 V1 O2 78.08(5) 2 15_556 ?
O4 V1 O2 79.89(5) . 15_556 ?
O3 V1 O2 77.99(5) . 15_556 ?
O1 V1 V1 96.02(5) . 2 ?
O2 V1 V1 42.94(4) . 2 ?
O2 V1 V1 40.83(4) 2 2 ?
O4 V1 V1 136.22(4) . 2 ?
O3 V1 V1 127.78(4) . 2 ?
O2 V1 V1 85.95(3) 15_556 2 ?
V1 O2 V1 96.23(6) . 2 ?
V1 O2 V1 102.00(6) . 16_556 ?
V1 O2 V1 99.73(6) 2 16_556 ?
P1 O3 V1 130.03(8) 15_556 . ?
P1 O4 V1 129.73(8) . . ?
O3 P1 O4 113.73(7) 16_556 . ?
O3 P1 C8 108.24(8) 16_556 . ?
O4 P1 C8 107.24(9) . . ?
O3 P1 C1 108.67(9) 16_556 . ?
O4 P1 C1 109.66(9) . . ?
C8 P1 C1 109.22(9) . . ?
C2 C1 P1 114.85(15) . . ?
C2 C1 H1A 108.6 . . ?
P1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
P1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.5 . . ?
C3 C2 C7 118.84(19) . . ?
C3 C2 C1 120.57(18) . . ?
C7 C2 C1 120.59(19) . . ?
C2 C3 C4 120.8(2) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C7 120.1(2) . . ?
C5 C6 H6 120 . . ?
C7 C6 H6 120 . . ?
C6 C7 C2 120.2(2) . . ?
C6 C7 H7 119.9 . . ?
C2 C7 H7 119.9 . . ?
C9 C8 P1 116.00(14) . . ?
C9 C8 H8A 108.3 . . ?
P1 C8 H8A 108.3 . . ?
C9 C8 H8B 108.3 . . ?
P1 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
C10 C9 C14 118.26(18) . . ?
C10 C9 C8 119.02(17) . . ?
C14 C9 C8 122.71(17) . . ?
C9 C10 C11 120.9(2) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C12 C11 C10 120.2(2) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 119.4(2) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 120.3(2) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C13 C14 C9 120.80(19) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF

_chemical_name_common            
;Tetrakisdibenzylphosphinato-octaoxo-
tetravanadium(V).tetrahydrate
;

# Attachment '- Tungsten.cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2011-06-25 at 13:09:32
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.4
# Request file : c:\wingx\files\archive.reqdat
# CIF files read : 11mz143_0m dreduc sadabs struct

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

data_11mz143_0m
_database_code_depnum_ccdc_archive 'CCDC 834512'
#TrackingRef '- Tungsten.cif'

_audit_creation_date             2011-06-25T13:09:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
Tetrakisdibenzylphosphinato-octaoxo-tetratungsten(V).tristetrahydrofuran
;
_chemical_formula_moiety         'C56 H56 O16 P4 W4, 3(C4 H8 O)'
_chemical_formula_sum            'C68 H80 O19 P4 W4 '
_chemical_formula_weight         2060.56
_chemical_compound_source        'synthesis as described'

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

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_Int_Tables_number      88
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   22.771(4)
_cell_length_b                   22.771(4)
_cell_length_c                   13.107(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6796(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9959
_cell_measurement_theta_min      2.5299
_cell_measurement_theta_max      30.9615
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.21
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3984
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    6.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_T_max  0.746

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

_diffrn_source                   'sealed x-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'APEX-II CCD'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_ub_11      0.336537E-1
_diffrn_orient_matrix_ub_12      0.243559E-1
_diffrn_orient_matrix_ub_13      -0.247442E-1
_diffrn_orient_matrix_ub_21      0.21986E-1
_diffrn_orient_matrix_ub_22      -0.874432E-2
_diffrn_orient_matrix_ub_23      0.642765E-1
_diffrn_orient_matrix_ub_31      0.176827E-1
_diffrn_orient_matrix_ub_32      -0.354818E-1
_diffrn_orient_matrix_ub_33      -0.328259E-1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_number            17299
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         31.11
_diffrn_reflns_theta_full        28
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.929
_reflns_number_total             5083
_reflns_number_gt                4522
_reflns_threshold_expression     >2\s(I)

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

_computing_data_collection       'Bruker APEX2 software'
_computing_cell_refinement       'SAINT V7.66A integration software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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   geom

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

_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^ > 2\s(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^)+(0.0167P)^2^+16.8014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5083
_refine_ls_number_parameters     243
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0189
_refine_ls_wR_factor_ref         0.0457
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.959
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.107

#----------------------------------------------------------------------------#
# 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
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
W1 W 0.968888(4) 0.201208(4) 0.016427(7) 0.01325(3) Uani 1 1 d . . .
O1 O 0.96255(8) 0.19135(8) -0.11139(14) 0.0195(3) Uani 1 1 d . . .
O2 O 0.94824(7) 0.28306(7) 0.05342(14) 0.0145(3) Uani 1 1 d . . .
O3 O 0.88282(7) 0.18561(7) 0.05407(13) 0.0163(3) Uani 1 1 d . . .
O4 O 0.98931(7) 0.11480(7) 0.05177(13) 0.0168(3) Uani 1 1 d . . .
P1 P 0.83861(3) 0.22588(3) 0.10916(5) 0.01497(11) Uani 1 1 d . . .
C1 C 0.80786(11) 0.27522(11) 0.0164(2) 0.0197(5) Uani 1 1 d . . .
H1A H 0.8404 0.2982 -0.014 0.024 Uiso 1 1 calc R . .
H1B H 0.7902 0.2514 -0.0389 0.024 Uiso 1 1 calc R . .
C2 C 0.76188(11) 0.31780(11) 0.0543(2) 0.0194(5) Uani 1 1 d . . .
C3 C 0.77848(12) 0.37186(11) 0.0951(2) 0.0260(6) Uani 1 1 d . . .
H3 H 0.819 0.3808 0.1032 0.031 Uiso 1 1 calc R . .
C4 C 0.73648(15) 0.41290(13) 0.1240(2) 0.0337(7) Uani 1 1 d . . .
H4 H 0.7483 0.4497 0.151 0.04 Uiso 1 1 calc R . .
C5 C 0.67721(14) 0.40004(14) 0.1133(2) 0.0337(7) Uani 1 1 d . . .
H5 H 0.6485 0.4284 0.1314 0.04 Uiso 1 1 calc R . .
C6 C 0.66010(13) 0.34588(15) 0.0762(2) 0.0328(7) Uani 1 1 d . . .
H6 H 0.6196 0.3365 0.0714 0.039 Uiso 1 1 calc R . .
C7 C 0.70199(12) 0.30525(13) 0.0461(2) 0.0251(5) Uani 1 1 d . . .
H7 H 0.6898 0.2684 0.0196 0.03 Uiso 1 1 calc R . .
C8 C 0.78176(10) 0.17941(11) 0.1585(2) 0.0186(5) Uani 1 1 d . . .
H8A H 0.7999 0.1504 0.2053 0.022 Uiso 1 1 calc R . .
H8B H 0.7546 0.2038 0.1994 0.022 Uiso 1 1 calc R . .
C9 C 0.74616(10) 0.14629(10) 0.0790(2) 0.0177(4) Uani 1 1 d . . .
C10 C 0.68529(11) 0.15050(12) 0.0810(2) 0.0257(6) Uani 1 1 d . . .
H10 H 0.6668 0.1737 0.132 0.031 Uiso 1 1 calc R . .
C11 C 0.65112(13) 0.12122(15) 0.0093(3) 0.0360(7) Uani 1 1 d . . .
H11 H 0.6096 0.1245 0.0116 0.043 Uiso 1 1 calc R . .
C12 C 0.67751(14) 0.08740(14) -0.0652(2) 0.0342(7) Uani 1 1 d . . .
H12 H 0.6542 0.0677 -0.1146 0.041 Uiso 1 1 calc R . .
C13 C 0.73802(13) 0.08241(12) -0.0676(2) 0.0281(6) Uani 1 1 d . . .
H13 H 0.7563 0.0588 -0.1183 0.034 Uiso 1 1 calc R . .
C14 C 0.77228(12) 0.11181(12) 0.0039(2) 0.0235(5) Uani 1 1 d . . .
H14 H 0.8138 0.1083 0.0015 0.028 Uiso 1 1 calc R . .
O5 O 0.4668(5) 0.4636(6) -0.0656(9) 0.036(4) Uani 0.238(14) 1 d P . .
C15 C 0.5173(4) 0.4517(3) -0.0240(4) 0.087(2) Uani 0.48(3) 1 d P . .
H15A H 0.5406 0.4285 -0.0733 0.104 Uiso 0.48(3) 1 calc PR . .
H15B H 0.5102 0.4264 0.0362 0.104 Uiso 0.48(3) 1 calc PR . .
C16 C 0.55211(19) 0.5006(3) 0.0080(4) 0.0694(15) Uani 0.48(3) 1 d P . .
H16A H 0.5883 0.4845 0.0392 0.083 Uiso 0.48(3) 1 calc PR . .
H16B H 0.5643 0.5218 -0.0544 0.083 Uiso 0.48(3) 1 calc PR . .
O51 O 0.4749(6) 0.4509(7) 0.000(2) 0.083(8) Uani 0.262(14) 1 d P . -1
C151 C 0.5173(4) 0.4517(3) -0.0240(4) 0.087(2) Uani 0.52(3) 1 d P . -1
H15C H 0.5171 0.4508 -0.0995 0.104 Uiso 0.52(3) 1 calc PR . -1
H15D H 0.5368 0.4153 -0.0003 0.104 Uiso 0.52(3) 1 calc PR . -1
C161 C 0.55211(19) 0.5006(3) 0.0080(4) 0.0694(15) Uani 0.52(3) 1 d P . -1
H16C H 0.5792 0.5152 -0.0454 0.083 Uiso 0.52(3) 1 calc PR . -1
H16D H 0.5734 0.4937 0.0728 0.083 Uiso 0.52(3) 1 calc PR . -1
O6 O 0.4701(10) 0.3095(9) -0.1358(13) 0.076(5) Uani 0.25 1 d PD . .
C17 C 0.5121(7) 0.2984(4) -0.1119(6) 0.100(2) Uani 1 1 d D . .
H17A H 0.5135(17) 0.305(2) -0.0368(15) 0.12 Uiso 1 1 d D . .
H17B H 0.5376(16) 0.3300(19) -0.141(3) 0.12 Uiso 1 1 d 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
W1 0.01349(5) 0.01334(5) 0.01291(5) -0.00055(3) -0.00026(3) -0.00011(3)
O1 0.0222(8) 0.0195(8) 0.0168(9) -0.0003(7) -0.0005(7) -0.0007(7)
O2 0.0153(7) 0.0156(7) 0.0125(8) 0.0004(6) -0.0004(6) -0.0006(6)
O3 0.0162(7) 0.0169(8) 0.0157(9) -0.0019(6) 0.0009(6) 0.0002(6)
O4 0.0182(8) 0.0154(7) 0.0167(8) 0.0010(6) -0.0018(6) -0.0011(6)
P1 0.0141(2) 0.0155(3) 0.0153(3) 0.0001(2) -0.0003(2) 0.0001(2)
C1 0.0212(11) 0.0205(11) 0.0175(12) 0.0010(9) 0.0000(9) 0.0008(9)
C2 0.0216(11) 0.0200(11) 0.0165(12) 0.0044(9) -0.0009(9) 0.0023(9)
C3 0.0263(13) 0.0205(12) 0.0311(16) 0.0036(10) 0.0075(11) -0.0031(10)
C4 0.0453(17) 0.0229(13) 0.0328(17) 0.0031(11) 0.0106(13) 0.0054(12)
C5 0.0373(16) 0.0366(16) 0.0273(16) 0.0091(12) 0.0047(12) 0.0191(13)
C6 0.0210(12) 0.0501(18) 0.0273(16) 0.0039(13) -0.0035(11) 0.0100(12)
C7 0.0226(12) 0.0318(14) 0.0210(13) 0.0022(11) -0.0049(10) 0.0031(10)
C8 0.0164(10) 0.0203(11) 0.0191(12) -0.0011(9) 0.0018(9) -0.0015(9)
C9 0.0170(10) 0.0175(10) 0.0184(12) 0.0015(9) 0.0004(9) -0.0019(8)
C10 0.0171(11) 0.0269(13) 0.0333(16) -0.0051(11) 0.0016(10) 0.0017(10)
C11 0.0218(13) 0.0392(17) 0.047(2) -0.0072(14) -0.0097(12) 0.0002(12)
C12 0.0354(16) 0.0360(16) 0.0310(17) -0.0023(12) -0.0100(13) -0.0084(13)
C13 0.0334(14) 0.0254(13) 0.0254(15) -0.0053(11) 0.0034(11) -0.0071(11)
C14 0.0206(12) 0.0229(12) 0.0268(14) -0.0033(10) 0.0036(10) -0.0026(10)
O5 0.026(5) 0.066(8) 0.017(6) 0.015(5) -0.010(4) -0.016(5)
C15 0.153(7) 0.061(3) 0.047(3) -0.006(2) -0.009(4) 0.001(4)
C16 0.036(2) 0.107(4) 0.065(3) 0.024(3) 0.008(2) -0.003(2)
O51 0.038(7) 0.072(10) 0.14(2) 0.011(10) -0.031(9) -0.029(7)
C151 0.153(7) 0.061(3) 0.047(3) -0.006(2) -0.009(4) 0.001(4)
C161 0.036(2) 0.107(4) 0.065(3) 0.024(3) 0.008(2) -0.003(2)
O6 0.067(10) 0.103(15) 0.059(9) 0.015(9) 0.004(7) 0.025(10)
C17 0.144(7) 0.088(5) 0.069(5) 0.001(4) 0.037(5) -0.029(5)

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

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
W1 O1 1.6964(19) . ?
W1 O2 1.9809(16) 2_755 ?
W1 O2 1.9825(16) . ?
W1 O3 2.0521(17) . ?
W1 O4 2.0742(17) . ?
W1 O2 2.3626(19) 16_645 ?
W1 W1 2.6354(5) 2_755 ?
O2 W1 1.9809(16) 2_755 ?
O2 W1 2.3626(19) 15_665 ?
O3 P1 1.5413(17) . ?
O4 P1 1.5320(18) 16_645 ?
P1 O4 1.5320(18) 15_665 ?
P1 C8 1.793(2) . ?
P1 C1 1.798(3) . ?
C1 C2 1.511(3) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 C3 1.394(4) . ?
C2 C7 1.398(4) . ?
C3 C4 1.390(4) . ?
C3 H3 0.95 . ?
C4 C5 1.388(5) . ?
C4 H4 0.95 . ?
C5 C6 1.381(5) . ?
C5 H5 0.95 . ?
C6 C7 1.386(4) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 C9 1.521(3) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 C10 1.390(3) . ?
C9 C14 1.392(4) . ?
C10 C11 1.390(4) . ?
C10 H10 0.95 . ?
C11 C12 1.382(5) . ?
C11 H11 0.95 . ?
C12 C13 1.383(4) . ?
C12 H12 0.95 . ?
C13 C14 1.392(4) . ?
C13 H13 0.95 . ?
C14 H14 0.95 . ?
O5 O51 0.93(2) . ?
O5 C16 1.191(13) 9_665 ?
O5 C161 1.191(13) 9_665 ?
O5 C15 1.301(14) . ?
C15 C16 1.431(8) . ?
C15 C16 1.928(9) 9_665 ?
C15 C161 1.928(9) 9_665 ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 O5 1.191(13) 9_665 ?
C16 C15 1.928(9) 9_665 ?
C16 C151 1.928(9) 9_665 ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
O51 C151 1.017(15) . ?
O51 C16 1.268(17) 9_665 ?
C151 C161 1.431(8) . ?
C151 C16 1.928(9) 9_665 ?
C151 H15C 0.99 . ?
C151 H15D 0.99 . ?
C161 C15 1.928(9) 9_665 ?
C161 H16C 0.99 . ?
C161 H16D 0.99 . ?
O6 C17 1.038(16) . ?
O6 C17 1.16(2) 12_655 ?
C17 O6 1.16(2) 11_665 ?
C17 C17 1.644(10) 12_655 ?
C17 C17 1.644(10) 11_665 ?
C17 H17A 0.996(18) . ?
C17 H17B 1.001(18) . ?

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 W1 O2 110.29(8) . 2_755 ?
O1 W1 O2 110.23(8) . . ?
O2 W1 O2 89.77(7) 2_755 . ?
O1 W1 O3 97.66(8) . . ?
O2 W1 O3 151.91(8) 2_755 . ?
O2 W1 O3 82.96(6) . . ?
O1 W1 O4 96.55(8) . . ?
O2 W1 O4 84.45(6) 2_755 . ?
O2 W1 O4 152.92(8) . . ?
O3 W1 O4 89.78(6) . . ?
O1 W1 O2 168.99(7) . 16_645 ?
O2 W1 O2 77.20(6) 2_755 16_645 ?
O2 W1 O2 77.17(6) . 16_645 ?
O3 W1 O2 74.74(6) . 16_645 ?
O4 W1 O2 75.76(6) . 16_645 ?
O1 W1 W1 99.05(6) . 2_755 ?
O2 W1 W1 48.35(5) 2_755 2_755 ?
O2 W1 W1 48.30(5) . 2_755 ?
O3 W1 W1 131.26(5) . 2_755 ?
O4 W1 W1 132.79(5) . 2_755 ?
O2 W1 W1 91.96(4) 16_645 2_755 ?
W1 O2 W1 83.35(6) 2_755 . ?
W1 O2 W1 102.76(7) 2_755 15_665 ?
W1 O2 W1 102.71(7) . 15_665 ?
P1 O3 W1 129.30(10) . . ?
P1 O4 W1 130.95(10) 16_645 . ?
O4 P1 O3 114.25(10) 15_665 . ?
O4 P1 C8 108.14(11) 15_665 . ?
O3 P1 C8 106.82(10) . . ?
O4 P1 C1 110.11(11) 15_665 . ?
O3 P1 C1 108.02(11) . . ?
C8 P1 C1 109.39(12) . . ?
C2 C1 P1 116.61(18) . . ?
C2 C1 H1A 108.1 . . ?
P1 C1 H1A 108.1 . . ?
C2 C1 H1B 108.1 . . ?
P1 C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C3 C2 C7 118.3(2) . . ?
C3 C2 C1 120.3(2) . . ?
C7 C2 C1 121.3(2) . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120 . . ?
C3 C4 H4 120 . . ?
C6 C5 C4 119.9(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.1(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C2 120.9(3) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
C9 C8 P1 115.46(18) . . ?
C9 C8 H8A 108.4 . . ?
P1 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
P1 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
C10 C9 C14 118.6(2) . . ?
C10 C9 C8 119.0(2) . . ?
C14 C9 C8 122.4(2) . . ?
C9 C10 C11 120.8(3) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 119.7(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C14 120.2(3) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C9 120.5(3) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
O51 O5 C16 72.2(14) . 9_665 ?
O51 O5 C161 72.2(14) . 9_665 ?
C16 O5 C161 0.0(8) 9_665 9_665 ?
O51 O5 C15 51.0(12) . . ?
C16 O5 C15 101.3(9) 9_665 . ?
C161 O5 C15 101.3(9) 9_665 . ?
O5 C15 C16 116.8(7) . . ?
O5 C15 C16 37.3(6) . 9_665 ?
C16 C15 C16 89.1(4) . 9_665 ?
O5 C15 C161 37.3(6) . 9_665 ?
C16 C15 C161 89.1(4) . 9_665 ?
C16 C15 C161 0.0(4) 9_665 9_665 ?
O5 C15 H15A 108.1 . . ?
C16 C15 H15A 108.1 . . ?
C16 C15 H15A 144.2 9_665 . ?
C161 C15 H15A 144.2 9_665 . ?
O5 C15 H15B 108.1 . . ?
C16 C15 H15B 108.1 . . ?
C16 C15 H15B 96.1 9_665 . ?
C161 C15 H15B 96.1 9_665 . ?
H15A C15 H15B 107.3 . . ?
O5 C16 C15 121.2(6) 9_665 . ?
O5 C16 C15 41.4(6) 9_665 9_665 ?
C15 C16 C15 90.9(4) . 9_665 ?
O5 C16 C151 41.4(6) 9_665 9_665 ?
C15 C16 C151 90.9(4) . 9_665 ?
C15 C16 C151 0.0(4) 9_665 9_665 ?
O5 C16 H16A 107 9_665 . ?
C15 C16 H16A 107 . . ?
C15 C16 H16A 147.8 9_665 . ?
C151 C16 H16A 147.8 9_665 . ?
O5 C16 H16B 107 9_665 . ?
C15 C16 H16B 107 . . ?
C15 C16 H16B 92.7 9_665 . ?
C151 C16 H16B 92.7 9_665 . ?
H16A C16 H16B 106.8 . . ?
O5 O51 C151 84(2) . . ?
O5 O51 C16 63.4(13) . 9_665 ?
C151 O51 C16 114.6(16) . 9_665 ?
O51 C151 C161 116.7(12) . . ?
O51 C151 C16 36.7(11) . 9_665 ?
C161 C151 C16 89.1(4) . 9_665 ?
O51 C151 H15C 108.1 . . ?
C161 C151 H15C 108.1 . . ?
C16 C151 H15C 96.7 9_665 . ?
O51 C151 H15D 108.1 . . ?
C161 C151 H15D 108.1 . . ?
C16 C151 H15D 143.6 9_665 . ?
H15C C151 H15D 107.3 . . ?
C151 C161 C15 90.9(4) . 9_665 ?
C151 C161 H16C 113.5 . . ?
C15 C161 H16C 113.5 9_665 . ?
C151 C161 H16D 113.5 . . ?
C15 C161 H16D 113.5 9_665 . ?
H16C C161 H16D 110.8 . . ?
C17 O6 C17 96.8(16) . 12_655 ?
O6 C17 O6 159.9(11) . 11_665 ?
O6 C17 C17 44.4(12) . 12_655 ?
O6 C17 C17 126.3(9) 11_665 12_655 ?
O6 C17 C17 127.1(13) . 11_665 ?
O6 C17 C17 38.8(9) 11_665 11_665 ?
C17 C17 C17 87.5(2) 12_655 11_665 ?
O6 C17 H17A 107(2) . . ?
O6 C17 H17A 93(2) 11_665 . ?
C17 C17 H17A 108(3) 12_655 . ?
C17 C17 H17A 108(3) 11_665 . ?
O6 C17 H17B 104(2) . . ?
O6 C17 H17B 73(3) 11_665 . ?
C17 C17 H17B 140(3) 12_655 . ?
C17 C17 H17B 103(3) 11_665 . ?
H17A C17 H17B 105(2) . . ?
_chemical_name_common            
;Tetrakisdibenzylphosphinato-octaoxo-
tetratungsten(V).tristetrahydrofuran
;