# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_2128
_database_code_depnum_ccdc_archive 'CCDC 1423351'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H21 Cr O6 P'
_chemical_formula_sum            'C31 H21 Cr O6 P'
_chemical_formula_weight         572.45
_chemical_absolute_configuration .

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'
Cr Cr 0.3209 0.6236 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   8.5858(5)
_cell_length_b                   19.6165(9)
_cell_length_c                   15.6007(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2627.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    5244
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      29.38

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_type   Integration
_exptl_absorpt_correction_T_min  0.9232
_exptl_absorpt_correction_T_max  0.9787
_exptl_absorpt_process_details   'STOE XRed'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14343
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_sigmaI/netI    0.1707
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         28.00
_reflns_number_total             6334
_reflns_number_gt                3818
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         6334
_refine_ls_number_parameters     356
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0567
_refine_ls_wR_factor_gt          0.0495
_refine_ls_goodness_of_fit_ref   0.623
_refine_ls_restrained_S_all      0.624
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

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
C1 C 0.9203(3) 0.37060(15) 0.23786(19) 0.0155(7) Uani 1 1 d . . .
H1 H 0.968(3) 0.4106(14) 0.223(2) 0.019 Uiso 1 1 d . . .
C2 C 0.9584(3) 0.34331(15) 0.3237(2) 0.0180(7) Uani 1 1 d . . .
C3 C 0.8802(3) 0.36651(16) 0.3958(2) 0.0219(8) Uani 1 1 d . . .
H3A H 0.7989 0.3990 0.3901 0.026 Uiso 1 1 calc R . .
C4 C 0.9206(4) 0.34237(18) 0.4762(2) 0.0302(8) Uani 1 1 d . . .
H4A H 0.8668 0.3583 0.5255 0.036 Uiso 1 1 calc R . .
C5 C 1.0377(4) 0.29568(17) 0.4847(2) 0.0304(9) Uani 1 1 d . . .
H5A H 1.0648 0.2792 0.5400 0.036 Uiso 1 1 calc R . .
C6 C 1.1170(3) 0.2723(2) 0.4136(2) 0.0319(8) Uani 1 1 d . . .
H6A H 1.1983 0.2398 0.4197 0.038 Uiso 1 1 calc R . .
C7 C 1.0770(3) 0.29642(17) 0.3332(2) 0.0285(8) Uani 1 1 d . . .
H7A H 1.1317 0.2806 0.2841 0.034 Uiso 1 1 calc R . .
C8 C 0.7115(3) 0.43043(14) 0.1119(2) 0.0135(7) Uani 1 1 d . . .
C9 C 0.6370(3) 0.41254(15) 0.02439(19) 0.0124(6) Uani 1 1 d . . .
C10 C 0.6513(3) 0.34885(17) -0.0132(2) 0.0196(7) Uani 1 1 d . . .
H10A H 0.7033 0.3136 0.0172 0.024 Uiso 1 1 calc R . .
C11 C 0.5919(3) 0.33515(17) -0.0939(2) 0.0229(8) Uani 1 1 d . . .
H11A H 0.6014 0.2908 -0.1178 0.027 Uiso 1 1 calc R . .
C12 C 0.5184(3) 0.38672(18) -0.1397(2) 0.0236(8) Uani 1 1 d . . .
H12A H 0.4765 0.3779 -0.1950 0.028 Uiso 1 1 calc R . .
C13 C 0.5072(3) 0.45034(17) -0.1041(2) 0.0205(8) Uani 1 1 d . . .
H13A H 0.4587 0.4860 -0.1354 0.025 Uiso 1 1 calc R . .
C14 C 0.5658(3) 0.46328(15) -0.02278(19) 0.0165(7) Uani 1 1 d . . .
H14A H 0.5568 0.5078 0.0008 0.020 Uiso 1 1 calc R . .
C15 C 0.6019(3) 0.46808(14) 0.1739(2) 0.0135(6) Uani 1 1 d . . .
C16 C 0.4408(3) 0.47205(14) 0.16105(19) 0.0172(6) Uani 1 1 d . . .
H16A H 0.3963 0.4527 0.1109 0.021 Uiso 1 1 calc R . .
C17 C 0.3453(3) 0.50393(16) 0.2207(2) 0.0225(7) Uani 1 1 d . . .
H17A H 0.2366 0.5071 0.2102 0.027 Uiso 1 1 calc R . .
C18 C 0.4062(3) 0.53094(15) 0.2948(2) 0.0221(8) Uani 1 1 d . . .
H18A H 0.3401 0.5523 0.3356 0.026 Uiso 1 1 calc R . .
C19 C 0.5657(4) 0.52665(15) 0.30928(18) 0.0201(7) Uani 1 1 d . . .
H19A H 0.6092 0.5452 0.3602 0.024 Uiso 1 1 calc R . .
C20 C 0.6606(3) 0.49556(15) 0.25005(19) 0.0154(7) Uani 1 1 d . . .
H20A H 0.7691 0.4927 0.2612 0.018 Uiso 1 1 calc R . .
C21 C 0.8593(3) 0.47071(15) 0.0888(2) 0.0137(7) Uani 1 1 d . . .
C22 C 0.9839(3) 0.43873(16) 0.0473(2) 0.0166(7) Uani 1 1 d . . .
H22A H 0.9793 0.3911 0.0364 0.020 Uiso 1 1 calc R . .
C23 C 1.1133(3) 0.47514(17) 0.0219(2) 0.0195(7) Uani 1 1 d . . .
H23A H 1.1979 0.4522 -0.0046 0.023 Uiso 1 1 calc R . .
C24 C 1.1208(4) 0.54437(17) 0.0346(2) 0.0239(8) Uani 1 1 d . . .
H24A H 1.2096 0.5693 0.0164 0.029 Uiso 1 1 calc R . .
C25 C 0.9986(4) 0.57721(17) 0.0739(2) 0.0224(8) Uani 1 1 d . . .
H25A H 1.0027 0.6252 0.0821 0.027 Uiso 1 1 calc R . .
C26 C 0.8694(3) 0.54095(16) 0.1018(2) 0.0176(7) Uani 1 1 d . . .
H26A H 0.7870 0.5642 0.1300 0.021 Uiso 1 1 calc R . .
C27 C 0.6167(3) 0.21476(17) 0.1281(2) 0.0212(8) Uani 1 1 d . . .
C28 C 0.7061(3) 0.22659(18) 0.2884(2) 0.0209(7) Uani 1 1 d U . .
C29 C 0.4156(3) 0.20836(15) 0.2599(2) 0.0208(7) Uani 1 1 d U . .
C30 C 0.3958(3) 0.30796(16) 0.1474(2) 0.0216(7) Uani 1 1 d U . .
C31 C 0.4964(3) 0.33224(16) 0.3113(2) 0.0200(8) Uani 1 1 d . . .
Cr Cr 0.55712(5) 0.27272(3) 0.21965(3) 0.01557(10) Uani 1 1 d U . .
O1 O 0.9266(2) 0.32269(10) 0.16422(13) 0.0186(5) Uani 1 1 d . . .
O2 O 0.6492(3) 0.17864(12) 0.07365(16) 0.0353(6) Uani 1 1 d . . .
O3 O 0.7878(2) 0.19277(12) 0.32638(17) 0.0363(7) Uani 1 1 d . . .
O4 O 0.3311(2) 0.16833(11) 0.28745(17) 0.0320(6) Uani 1 1 d U . .
O5 O 0.2948(2) 0.32361(12) 0.10557(17) 0.0334(6) Uani 1 1 d . . .
O6 O 0.4592(3) 0.36550(12) 0.36675(16) 0.0358(6) Uani 1 1 d . . .
P P 0.74672(9) 0.35171(4) 0.17955(5) 0.01370(16) Uani 1 1 d . . .


_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
C1 C2 1.478(4) . ?
C1 O1 1.485(3) . ?
C1 P 1.785(3) . ?
C1 H1 0.92(3) . ?
C2 C7 1.381(4) . ?
C2 C3 1.387(4) . ?
C3 C4 1.385(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.366(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.381(5) . ?
C5 H5A 0.9500 . ?
C6 C7 1.384(4) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C21 1.538(4) . ?
C8 C15 1.538(4) . ?
C8 C9 1.548(4) . ?
C8 P 1.895(3) . ?
C9 C14 1.380(4) . ?
C9 C10 1.386(4) . ?
C10 C11 1.384(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.390(4) . ?
C11 H11A 0.9500 . ?
C12 C13 1.370(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.388(4) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C20 1.398(4) . ?
C15 C16 1.400(4) . ?
C16 C17 1.389(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.375(4) . ?
C17 H17A 0.9500 . ?
C18 C19 1.391(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.374(4) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
C21 C26 1.395(4) . ?
C21 C22 1.399(4) . ?
C22 C23 1.379(4) . ?
C22 H22A 0.9500 . ?
C23 C24 1.374(4) . ?
C23 H23A 0.9500 . ?
C24 C25 1.376(4) . ?
C24 H24A 0.9500 . ?
C25 C26 1.387(4) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 O2 1.141(4) . ?
C27 Cr 1.895(3) . ?
C28 O3 1.133(3) . ?
C28 Cr 1.899(3) . ?
C29 O4 1.152(3) . ?
C29 Cr 1.861(3) . ?
C30 O5 1.128(3) . ?
C30 Cr 1.915(3) . ?
C31 O6 1.129(4) . ?
C31 Cr 1.919(3) . ?
Cr P 2.3328(9) . ?
O1 P 1.663(2) . ?

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
C2 C1 O1 117.6(2) . . ?
C2 C1 P 124.8(2) . . ?
O1 C1 P 60.30(13) . . ?
C2 C1 H1 117(2) . . ?
O1 C1 H1 109(2) . . ?
P C1 H1 114.7(18) . . ?
C7 C2 C3 119.2(3) . . ?
C7 C2 C1 120.1(3) . . ?
C3 C2 C1 120.6(3) . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
C5 C6 C7 119.5(3) . . ?
C5 C6 H6A 120.2 . . ?
C7 C6 H6A 120.2 . . ?
C2 C7 C6 120.6(3) . . ?
C2 C7 H7A 119.7 . . ?
C6 C7 H7A 119.7 . . ?
C21 C8 C15 113.9(2) . . ?
C21 C8 C9 104.5(2) . . ?
C15 C8 C9 114.3(2) . . ?
C21 C8 P 114.68(19) . . ?
C15 C8 P 97.98(19) . . ?
C9 C8 P 111.9(2) . . ?
C14 C9 C10 117.6(3) . . ?
C14 C9 C8 119.3(3) . . ?
C10 C9 C8 122.8(3) . . ?
C11 C10 C9 121.8(3) . . ?
C11 C10 H10A 119.1 . . ?
C9 C10 H10A 119.1 . . ?
C10 C11 C12 119.6(3) . . ?
C10 C11 H11A 120.2 . . ?
C12 C11 H11A 120.2 . . ?
C13 C12 C11 119.1(3) . . ?
C13 C12 H12A 120.4 . . ?
C11 C12 H12A 120.4 . . ?
C12 C13 C14 120.8(3) . . ?
C12 C13 H13A 119.6 . . ?
C14 C13 H13A 119.6 . . ?
C9 C14 C13 121.0(3) . . ?
C9 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
C20 C15 C16 117.2(3) . . ?
C20 C15 C8 119.9(2) . . ?
C16 C15 C8 122.7(3) . . ?
C17 C16 C15 120.8(3) . . ?
C17 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 . . ?
C18 C17 C16 120.8(3) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C17 C18 C19 119.2(3) . . ?
C17 C18 H18A 120.4 . . ?
C19 C18 H18A 120.4 . . ?
C20 C19 C18 120.1(3) . . ?
C20 C19 H19A 120.0 . . ?
C18 C19 H19A 120.0 . . ?
C19 C20 C15 121.9(3) . . ?
C19 C20 H20A 119.0 . . ?
C15 C20 H20A 119.0 . . ?
C26 C21 C22 117.5(3) . . ?
C26 C21 C8 121.6(3) . . ?
C22 C21 C8 120.6(3) . . ?
C23 C22 C21 121.1(3) . . ?
C23 C22 H22A 119.4 . . ?
C21 C22 H22A 119.4 . . ?
C24 C23 C22 120.6(3) . . ?
C24 C23 H23A 119.7 . . ?
C22 C23 H23A 119.7 . . ?
C23 C24 C25 119.4(3) . . ?
C23 C24 H24A 120.3 . . ?
C25 C24 H24A 120.3 . . ?
C24 C25 C26 120.6(3) . . ?
C24 C25 H25A 119.7 . . ?
C26 C25 H25A 119.7 . . ?
C25 C26 C21 120.7(3) . . ?
C25 C26 H26A 119.6 . . ?
C21 C26 H26A 119.6 . . ?
O2 C27 Cr 178.0(3) . . ?
O3 C28 Cr 172.6(3) . . ?
O4 C29 Cr 177.5(3) . . ?
O5 C30 Cr 174.2(3) . . ?
O6 C31 Cr 177.8(3) . . ?
C29 Cr C27 91.34(13) . . ?
C29 Cr C28 85.75(12) . . ?
C27 Cr C28 87.59(14) . . ?
C29 Cr C30 88.35(13) . . ?
C27 Cr C30 88.19(14) . . ?
C28 Cr C30 172.66(14) . . ?
C29 Cr C31 89.09(13) . . ?
C27 Cr C31 179.33(15) . . ?
C28 Cr C31 92.95(14) . . ?
C30 Cr C31 91.31(14) . . ?
C29 Cr P 175.21(10) . . ?
C27 Cr P 90.46(9) . . ?
C28 Cr P 89.89(9) . . ?
C30 Cr P 96.14(9) . . ?
C31 Cr P 89.15(9) . . ?
C1 O1 P 68.83(14) . . ?
O1 P C1 50.88(11) . . ?
O1 P C8 110.31(11) . . ?
C1 P C8 104.35(14) . . ?
O1 P Cr 117.33(8) . . ?
C1 P Cr 125.73(11) . . ?
C8 P Cr 125.40(9) . . ?

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
O1 C1 C2 C7 38.8(4) . . . . ?
P C1 C2 C7 110.3(3) . . . . ?
O1 C1 C2 C3 -144.0(3) . . . . ?
P C1 C2 C3 -72.5(4) . . . . ?
C7 C2 C3 C4 -0.4(4) . . . . ?
C1 C2 C3 C4 -177.7(3) . . . . ?
C2 C3 C4 C5 0.1(5) . . . . ?
C3 C4 C5 C6 0.2(5) . . . . ?
C4 C5 C6 C7 0.0(5) . . . . ?
C3 C2 C7 C6 0.6(5) . . . . ?
C1 C2 C7 C6 177.8(3) . . . . ?
C5 C6 C7 C2 -0.3(5) . . . . ?
C21 C8 C9 C14 -72.6(3) . . . . ?
C15 C8 C9 C14 52.6(4) . . . . ?
P C8 C9 C14 162.8(2) . . . . ?
C21 C8 C9 C10 101.0(3) . . . . ?
C15 C8 C9 C10 -133.8(3) . . . . ?
P C8 C9 C10 -23.7(3) . . . . ?
C14 C9 C10 C11 -2.3(4) . . . . ?
C8 C9 C10 C11 -176.0(3) . . . . ?
C9 C10 C11 C12 1.3(4) . . . . ?
C10 C11 C12 C13 0.4(4) . . . . ?
C11 C12 C13 C14 -1.1(4) . . . . ?
C10 C9 C14 C13 1.6(4) . . . . ?
C8 C9 C14 C13 175.5(3) . . . . ?
C12 C13 C14 C9 0.0(4) . . . . ?
C21 C8 C15 C20 -51.0(4) . . . . ?
C9 C8 C15 C20 -171.0(3) . . . . ?
P C8 C15 C20 70.6(3) . . . . ?
C21 C8 C15 C16 134.0(3) . . . . ?
C9 C8 C15 C16 13.9(4) . . . . ?
P C8 C15 C16 -104.5(3) . . . . ?
C20 C15 C16 C17 1.9(4) . . . . ?
C8 C15 C16 C17 177.1(3) . . . . ?
C15 C16 C17 C18 -1.5(5) . . . . ?
C16 C17 C18 C19 0.6(5) . . . . ?
C17 C18 C19 C20 -0.2(5) . . . . ?
C18 C19 C20 C15 0.6(5) . . . . ?
C16 C15 C20 C19 -1.4(4) . . . . ?
C8 C15 C20 C19 -176.8(3) . . . . ?
C15 C8 C21 C26 -18.0(4) . . . . ?
C9 C8 C21 C26 107.4(3) . . . . ?
P C8 C21 C26 -129.8(3) . . . . ?
C15 C8 C21 C22 167.3(3) . . . . ?
C9 C8 C21 C22 -67.3(3) . . . . ?
P C8 C21 C22 55.6(3) . . . . ?
C26 C21 C22 C23 1.4(5) . . . . ?
C8 C21 C22 C23 176.3(3) . . . . ?
C21 C22 C23 C24 -2.0(5) . . . . ?
C22 C23 C24 C25 0.8(5) . . . . ?
C23 C24 C25 C26 0.9(5) . . . . ?
C24 C25 C26 C21 -1.4(5) . . . . ?
C22 C21 C26 C25 0.3(5) . . . . ?
C8 C21 C26 C25 -174.5(3) . . . . ?
O4 C29 Cr C27 116(6) . . . . ?
O4 C29 Cr C28 29(6) . . . . ?
O4 C29 Cr C30 -156(6) . . . . ?
O4 C29 Cr C31 -65(6) . . . . ?
O4 C29 Cr P 4(7) . . . . ?
O2 C27 Cr C29 9(9) . . . . ?
O2 C27 Cr C28 94(9) . . . . ?
O2 C27 Cr C30 -80(9) . . . . ?
O2 C27 Cr C31 -121(12) . . . . ?
O2 C27 Cr P -176(100) . . . . ?
O3 C28 Cr C29 42(2) . . . . ?
O3 C28 Cr C27 -50(2) . . . . ?
O3 C28 Cr C30 5(3) . . . . ?
O3 C28 Cr C31 131(2) . . . . ?
O3 C28 Cr P -140(2) . . . . ?
O5 C30 Cr C29 -21(3) . . . . ?
O5 C30 Cr C27 71(3) . . . . ?
O5 C30 Cr C28 16(4) . . . . ?
O5 C30 Cr C31 -110(3) . . . . ?
O5 C30 Cr P 161(3) . . . . ?
O6 C31 Cr C29 24(7) . . . . ?
O6 C31 Cr C27 153(10) . . . . ?
O6 C31 Cr C28 -62(7) . . . . ?
O6 C31 Cr C30 112(7) . . . . ?
O6 C31 Cr P -152(7) . . . . ?
C2 C1 O1 P 116.3(2) . . . . ?
C1 O1 P C8 92.27(18) . . . . ?
C1 O1 P Cr -115.27(14) . . . . ?
C2 C1 P O1 -104.7(3) . . . . ?
C2 C1 P C8 150.6(2) . . . . ?
O1 C1 P C8 -104.70(15) . . . . ?
C2 C1 P Cr -6.4(3) . . . . ?
O1 C1 P Cr 98.28(14) . . . . ?
C21 C8 P O1 -25.5(2) . . . . ?
C15 C8 P O1 -146.51(16) . . . . ?
C9 C8 P O1 93.3(2) . . . . ?
C21 C8 P C1 27.6(3) . . . . ?
C15 C8 P C1 -93.36(18) . . . . ?
C9 C8 P C1 146.43(19) . . . . ?
C21 C8 P Cr -175.24(17) . . . . ?
C15 C8 P Cr 63.8(2) . . . . ?
C9 C8 P Cr -56.5(2) . . . . ?
C29 Cr P O1 61.9(12) . . . . ?
C27 Cr P O1 -50.25(13) . . . . ?
C28 Cr P O1 37.34(13) . . . . ?
C30 Cr P O1 -138.48(13) . . . . ?
C31 Cr P O1 130.30(13) . . . . ?
C29 Cr P C1 2.1(12) . . . . ?
C27 Cr P C1 -110.04(15) . . . . ?
C28 Cr P C1 -22.45(16) . . . . ?
C30 Cr P C1 161.73(16) . . . . ?
C31 Cr P C1 70.51(16) . . . . ?
C29 Cr P C8 -150.3(11) . . . . ?
C27 Cr P C8 97.61(15) . . . . ?
C28 Cr P C8 -174.80(16) . . . . ?
C30 Cr P C8 9.38(16) . . . . ?
C31 Cr P C8 -81.84(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_2463-new2
_database_code_depnum_ccdc_archive 'CCDC 1423352'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H21 Mo O6 P'
_chemical_formula_sum            'C31 H21 Mo O6 P'
_chemical_formula_weight         616.39
_chemical_absolute_configuration ad
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'
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   8.6515(3)
_cell_length_b                   15.6935(4)
_cell_length_c                   19.9770(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2712.32(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    8559
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      29.36

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_type   Integration
_exptl_absorpt_correction_T_min  0.9437
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_process_details   'STOE XRed'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19516
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_sigmaI/netI    0.1091
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         28.00
_reflns_number_total             6550
_reflns_number_gt                5083
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0039P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(3)
_refine_ls_number_reflns         6550
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.0585
_refine_ls_wR_factor_gt          0.0549
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_restrained_S_all      0.840
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.1686(3) 0.9878(3) 0.1217(2) 0.0202(9) Uani 1 1 d . . .
H1 H 1.215(4) 0.977(3) 0.1613(18) 0.024 Uiso 1 1 d . . .
C2 C 1.2022(4) 1.0740(3) 0.09431(19) 0.0239(8) Uani 1 1 d . . .
C3 C 1.1234(4) 1.1450(3) 0.1172(2) 0.0275(10) Uani 1 1 d . . .
H3A H 1.0451 1.1385 0.1502 0.033 Uiso 1 1 calc R . .
C4 C 1.1567(5) 1.2245(3) 0.0930(3) 0.0352(11) Uani 1 1 d . . .
H4A H 1.1008 1.2726 0.1088 0.042 Uiso 1 1 calc R . .
C5 C 1.2714(5) 1.2348(3) 0.0458(2) 0.0397(12) Uani 1 1 d . . .
H5A H 1.2956 1.2900 0.0294 0.048 Uiso 1 1 calc R . .
C6 C 1.3516(4) 1.1642(3) 0.0223(3) 0.0407(11) Uani 1 1 d . . .
H6A H 1.4305 1.1709 -0.0103 0.049 Uiso 1 1 calc R . .
C7 C 1.3163(4) 1.0849(3) 0.0464(2) 0.0348(11) Uani 1 1 d . . .
H7A H 1.3709 1.0367 0.0301 0.042 Uiso 1 1 calc R . .
C8 C 0.9601(3) 0.8614(2) 0.1803(2) 0.0176(8) Uani 1 1 d . . .
C9 C 1.1089(4) 0.8397(2) 0.2207(2) 0.0175(8) Uani 1 1 d . . .
C10 C 1.2320(4) 0.7976(2) 0.1887(2) 0.0196(8) Uani 1 1 d . . .
H10A H 1.2263 0.7857 0.1422 0.024 Uiso 1 1 calc R . .
C11 C 1.3616(4) 0.7736(3) 0.2249(2) 0.0236(9) Uani 1 1 d . . .
H11A H 1.4459 0.7471 0.2026 0.028 Uiso 1 1 calc R . .
C12 C 1.3694(4) 0.7876(3) 0.2918(2) 0.0285(10) Uani 1 1 d . . .
H12A H 1.4583 0.7704 0.3163 0.034 Uiso 1 1 calc R . .
C13 C 1.2481(4) 0.8270(3) 0.3244(2) 0.0261(10) Uani 1 1 d . . .
H13A H 1.2531 0.8363 0.3714 0.031 Uiso 1 1 calc R . .
C14 C 1.1188(4) 0.8528(3) 0.2885(2) 0.0226(9) Uani 1 1 d . . .
H14 H 1.0359 0.8800 0.3112 0.027 Uiso 1 1 calc R . .
C15 C 0.8864(4) 0.7754(2) 0.1625(2) 0.0172(8) Uani 1 1 d . . .
C16 C 0.8962(4) 0.7390(3) 0.0996(2) 0.0236(9) Uani 1 1 d . . .
H16A H 0.9454 0.7695 0.0645 0.028 Uiso 1 1 calc R . .
C17 C 0.8358(4) 0.6592(3) 0.0869(2) 0.0298(11) Uani 1 1 d . . .
H17A H 0.8417 0.6361 0.0430 0.036 Uiso 1 1 calc R . .
C18 C 0.7672(4) 0.6128(3) 0.1372(2) 0.0298(11) Uani 1 1 d . . .
H18A H 0.7260 0.5579 0.1284 0.036 Uiso 1 1 calc R . .
C19 C 0.7592(4) 0.6471(3) 0.2005(2) 0.0254(10) Uani 1 1 d . . .
H19A H 0.7117 0.6156 0.2355 0.030 Uiso 1 1 calc R . .
C20 C 0.8193(4) 0.7268(2) 0.2138(2) 0.0200(8) Uani 1 1 d . . .
H20A H 0.8152 0.7490 0.2580 0.024 Uiso 1 1 calc R . .
C21 C 0.8516(4) 0.9240(3) 0.2179(2) 0.0177(8) Uani 1 1 d . . .
C22 C 0.9090(4) 0.9995(2) 0.2447(2) 0.0207(9) Uani 1 1 d . . .
H22A H 1.0167 1.0109 0.2420 0.025 Uiso 1 1 calc R . .
C23 C 0.8138(5) 1.0580(2) 0.2751(2) 0.0262(9) Uani 1 1 d . . .
H23A H 0.8566 1.1084 0.2939 0.031 Uiso 1 1 calc R . .
C24 C 0.6566(4) 1.0443(3) 0.2785(2) 0.0279(11) Uani 1 1 d . . .
H24A H 0.5905 1.0851 0.2987 0.033 Uiso 1 1 calc R . .
C25 C 0.5972(4) 0.9698(3) 0.2519(2) 0.0269(8) Uani 1 1 d . . .
H25A H 0.4894 0.9590 0.2552 0.032 Uiso 1 1 calc R . .
C26 C 0.6913(4) 0.9106(2) 0.22057(19) 0.0227(8) Uani 1 1 d . . .
H26A H 0.6475 0.8611 0.2009 0.027 Uiso 1 1 calc R . .
C27 C 0.6443(4) 1.0144(3) -0.0463(2) 0.0254(10) Uani 1 1 d . . .
C28 C 0.7307(4) 1.0695(3) 0.0844(2) 0.0241(9) Uani 1 1 d . . .
C29 C 0.6271(4) 0.8946(3) 0.0589(2) 0.0246(9) Uani 1 1 d . . .
C30 C 0.8601(4) 0.8769(3) -0.0404(2) 0.0274(10) Uani 1 1 d . . .
C31 C 0.9537(4) 1.0476(2) -0.0274(3) 0.0267(10) Uani 1 1 d . . .
O1 O 1.1758(3) 0.91554(17) 0.07534(14) 0.0243(6) Uani 1 1 d . . .
O2 O 0.5590(3) 1.0396(2) -0.08545(15) 0.0394(8) Uani 1 1 d . . .
O3 O 0.6910(4) 1.1236(2) 0.11806(17) 0.0453(8) Uani 1 1 d . . .
O4 O 0.5272(3) 0.8519(2) 0.07589(17) 0.0411(9) Uani 1 1 d . . .
O5 O 0.8959(4) 0.8233(2) -0.07625(18) 0.0435(9) Uani 1 1 d . . .
O6 O 1.0346(3) 1.0874(2) -0.05988(18) 0.0489(10) Uani 1 1 d . . .
P P 0.99658(10) 0.92974(6) 0.10393(5) 0.0178(2) Uani 1 1 d . . .
Mo Mo 0.79566(3) 0.97255(2) 0.021538(17) 0.01771(6) Uani 1 1 d . . .


_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
C1 O1 1.465(5) . ?
C1 C2 1.487(5) . ?
C1 P 1.781(3) . ?
C1 H1 0.91(4) . ?
C2 C3 1.385(6) . ?
C2 C7 1.386(5) . ?
C3 C4 1.368(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.379(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.388(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.369(6) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C15 1.534(5) . ?
C8 C21 1.553(5) . ?
C8 C9 1.556(5) . ?
C8 P 1.892(4) . ?
C9 C14 1.372(6) . ?
C9 C10 1.407(5) . ?
C10 C11 1.387(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.357(6) . ?
C11 H11A 0.9500 . ?
C12 C13 1.381(5) . ?
C12 H12A 0.9500 . ?
C13 C14 1.391(5) . ?
C13 H13A 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.384(6) . ?
C15 C20 1.403(5) . ?
C16 C17 1.380(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.375(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.377(6) . ?
C18 H18A 0.9500 . ?
C19 C20 1.381(6) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
C21 C22 1.393(5) . ?
C21 C26 1.404(5) . ?
C22 C23 1.374(5) . ?
C22 H22A 0.9500 . ?
C23 C24 1.378(5) . ?
C23 H23A 0.9500 . ?
C24 C25 1.383(6) . ?
C24 H24A 0.9500 . ?
C25 C26 1.384(5) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 O2 1.145(4) . ?
C27 Mo 1.996(4) . ?
C28 O3 1.136(5) . ?
C28 Mo 2.052(4) . ?
C29 O4 1.145(4) . ?
C29 Mo 2.044(4) . ?
C30 O5 1.148(5) . ?
C30 Mo 2.024(5) . ?
C31 O6 1.141(5) . ?
C31 Mo 2.052(4) . ?
O1 P 1.668(2) . ?
P Mo 2.4864(10) . ?

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 C1 C2 117.6(3) . . ?
O1 C1 P 60.92(17) . . ?
C2 C1 P 123.8(3) . . ?
O1 C1 H1 112(3) . . ?
C2 C1 H1 114(3) . . ?
P C1 H1 117(2) . . ?
C3 C2 C7 118.6(4) . . ?
C3 C2 C1 121.0(3) . . ?
C7 C2 C1 120.4(4) . . ?
C4 C3 C2 120.9(4) . . ?
C4 C3 H3A 119.6 . . ?
C2 C3 H3A 119.6 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C4 C5 C6 119.8(4) . . ?
C4 C5 H5A 120.1 . . ?
C6 C5 H5A 120.1 . . ?
C7 C6 C5 119.7(5) . . ?
C7 C6 H6A 120.2 . . ?
C5 C6 H6A 120.2 . . ?
C6 C7 C2 120.9(4) . . ?
C6 C7 H7A 119.5 . . ?
C2 C7 H7A 119.5 . . ?
C15 C8 C21 114.7(3) . . ?
C15 C8 C9 105.8(3) . . ?
C21 C8 C9 112.8(3) . . ?
C15 C8 P 112.4(3) . . ?
C21 C8 P 97.6(2) . . ?
C9 C8 P 113.8(2) . . ?
C14 C9 C10 118.1(3) . . ?
C14 C9 C8 122.0(3) . . ?
C10 C9 C8 119.5(3) . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C12 C11 C10 120.7(4) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C11 C12 C13 120.0(4) . . ?
C11 C12 H12A 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C12 C13 C14 119.9(4) . . ?
C12 C13 H13A 120.0 . . ?
C14 C13 H13A 120.0 . . ?
C9 C14 C13 121.1(4) . . ?
C9 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C16 C15 C20 117.7(4) . . ?
C16 C15 C8 123.3(4) . . ?
C20 C15 C8 118.7(4) . . ?
C17 C16 C15 121.2(4) . . ?
C17 C16 H16A 119.4 . . ?
C15 C16 H16A 119.4 . . ?
C18 C17 C16 120.6(4) . . ?
C18 C17 H17A 119.7 . . ?
C16 C17 H17A 119.7 . . ?
C17 C18 C19 119.1(4) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
C18 C19 C20 120.8(4) . . ?
C18 C19 H19A 119.6 . . ?
C20 C19 H19A 119.6 . . ?
C19 C20 C15 120.5(4) . . ?
C19 C20 H20A 119.7 . . ?
C15 C20 H20A 119.7 . . ?
C22 C21 C26 117.7(3) . . ?
C22 C21 C8 120.6(3) . . ?
C26 C21 C8 121.4(3) . . ?
C23 C22 C21 121.6(4) . . ?
C23 C22 H22A 119.2 . . ?
C21 C22 H22A 119.2 . . ?
C22 C23 C24 120.6(4) . . ?
C22 C23 H23A 119.7 . . ?
C24 C23 H23A 119.7 . . ?
C23 C24 C25 118.7(4) . . ?
C23 C24 H24A 120.7 . . ?
C25 C24 H24A 120.7 . . ?
C24 C25 C26 121.5(3) . . ?
C24 C25 H25A 119.3 . . ?
C26 C25 H25A 119.3 . . ?
C25 C26 C21 119.9(4) . . ?
C25 C26 H26A 120.1 . . ?
C21 C26 H26A 120.1 . . ?
O2 C27 Mo 178.8(4) . . ?
O3 C28 Mo 177.9(4) . . ?
O4 C29 Mo 175.3(4) . . ?
O5 C30 Mo 179.0(4) . . ?
O6 C31 Mo 173.7(4) . . ?
C1 O1 P 68.93(16) . . ?
O1 P C1 50.16(14) . . ?
O1 P C8 110.82(14) . . ?
C1 P C8 105.61(17) . . ?
O1 P Mo 117.36(11) . . ?
C1 P Mo 125.28(14) . . ?
C8 P Mo 124.80(10) . . ?
C27 Mo C30 90.56(17) . . ?
C27 Mo C29 88.67(15) . . ?
C30 Mo C29 88.63(17) . . ?
C27 Mo C31 85.72(15) . . ?
C30 Mo C31 87.20(17) . . ?
C29 Mo C31 172.97(19) . . ?
C27 Mo C28 89.55(15) . . ?
C30 Mo C28 179.88(18) . . ?
C29 Mo C28 91.42(16) . . ?
C31 Mo C28 92.76(17) . . ?
C27 Mo P 175.72(12) . . ?
C30 Mo P 90.66(11) . . ?
C29 Mo P 95.46(11) . . ?
C31 Mo P 90.24(12) . . ?
C28 Mo P 89.23(11) . . ?

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
O1 C1 C2 C3 144.0(3) . . . . ?
P C1 C2 C3 72.1(5) . . . . ?
O1 C1 C2 C7 -37.7(5) . . . . ?
P C1 C2 C7 -109.6(4) . . . . ?
C7 C2 C3 C4 0.3(6) . . . . ?
C1 C2 C3 C4 178.6(4) . . . . ?
C2 C3 C4 C5 -0.8(7) . . . . ?
C3 C4 C5 C6 0.8(7) . . . . ?
C4 C5 C6 C7 -0.2(7) . . . . ?
C5 C6 C7 C2 -0.4(7) . . . . ?
C3 C2 C7 C6 0.4(7) . . . . ?
C1 C2 C7 C6 -178.0(4) . . . . ?
C15 C8 C9 C14 -107.3(4) . . . . ?
C21 C8 C9 C14 18.9(5) . . . . ?
P C8 C9 C14 128.8(4) . . . . ?
C15 C8 C9 C10 66.2(4) . . . . ?
C21 C8 C9 C10 -167.7(3) . . . . ?
P C8 C9 C10 -57.7(4) . . . . ?
C14 C9 C10 C11 -2.6(6) . . . . ?
C8 C9 C10 C11 -176.3(3) . . . . ?
C9 C10 C11 C12 2.3(6) . . . . ?
C10 C11 C12 C13 -0.7(6) . . . . ?
C11 C12 C13 C14 -0.6(6) . . . . ?
C10 C9 C14 C13 1.4(6) . . . . ?
C8 C9 C14 C13 174.9(4) . . . . ?
C12 C13 C14 C9 0.2(6) . . . . ?
C21 C8 C15 C16 132.1(4) . . . . ?
C9 C8 C15 C16 -103.0(4) . . . . ?
P C8 C15 C16 21.8(4) . . . . ?
C21 C8 C15 C20 -54.8(4) . . . . ?
C9 C8 C15 C20 70.2(4) . . . . ?
P C8 C15 C20 -165.0(2) . . . . ?
C20 C15 C16 C17 2.9(5) . . . . ?
C8 C15 C16 C17 176.1(3) . . . . ?
C15 C16 C17 C18 -1.5(6) . . . . ?
C16 C17 C18 C19 0.1(6) . . . . ?
C17 C18 C19 C20 -0.2(5) . . . . ?
C18 C19 C20 C15 1.7(5) . . . . ?
C16 C15 C20 C19 -3.0(5) . . . . ?
C8 C15 C20 C19 -176.5(3) . . . . ?
C15 C8 C21 C22 171.6(3) . . . . ?
C9 C8 C21 C22 50.4(5) . . . . ?
P C8 C21 C22 -69.5(4) . . . . ?
C15 C8 C21 C26 -14.4(5) . . . . ?
C9 C8 C21 C26 -135.7(4) . . . . ?
P C8 C21 C26 104.5(4) . . . . ?
C26 C21 C22 C23 2.3(6) . . . . ?
C8 C21 C22 C23 176.5(4) . . . . ?
C21 C22 C23 C24 -1.5(6) . . . . ?
C22 C23 C24 C25 1.2(6) . . . . ?
C23 C24 C25 C26 -1.8(7) . . . . ?
C24 C25 C26 C21 2.7(6) . . . . ?
C22 C21 C26 C25 -2.9(6) . . . . ?
C8 C21 C26 C25 -177.0(4) . . . . ?
C2 C1 O1 P -115.3(3) . . . . ?
C1 O1 P C8 -93.3(2) . . . . ?
C1 O1 P Mo 114.54(19) . . . . ?
C2 C1 P O1 105.4(4) . . . . ?
O1 C1 P C8 104.3(2) . . . . ?
C2 C1 P C8 -150.2(3) . . . . ?
O1 C1 P Mo -98.21(19) . . . . ?
C2 C1 P Mo 7.2(4) . . . . ?
C15 C8 P O1 -93.6(2) . . . . ?
C21 C8 P O1 145.7(2) . . . . ?
C9 C8 P O1 26.6(3) . . . . ?
C15 C8 P C1 -146.4(2) . . . . ?
C21 C8 P C1 93.0(2) . . . . ?
C9 C8 P C1 -26.1(3) . . . . ?
C15 C8 P Mo 56.0(3) . . . . ?
C21 C8 P Mo -64.6(2) . . . . ?
C9 C8 P Mo 176.3(2) . . . . ?
O2 C27 Mo C30 -109(19) . . . . ?
O2 C27 Mo C29 162(19) . . . . ?
O2 C27 Mo C31 -22(19) . . . . ?
O2 C27 Mo C28 71(19) . . . . ?
O2 C27 Mo P -3(20) . . . . ?
O5 C30 Mo C27 22(23) . . . . ?
O5 C30 Mo C29 111(23) . . . . ?
O5 C30 Mo C31 -63(23) . . . . ?
O5 C30 Mo C28 -134(100) . . . . ?
O5 C30 Mo P -154(23) . . . . ?
O4 C29 Mo C27 16(5) . . . . ?
O4 C29 Mo C30 -75(5) . . . . ?
O4 C29 Mo C31 -21(6) . . . . ?
O4 C29 Mo C28 106(5) . . . . ?
O4 C29 Mo P -165(5) . . . . ?
O6 C31 Mo C27 -35(3) . . . . ?
O6 C31 Mo C30 56(3) . . . . ?
O6 C31 Mo C29 2(4) . . . . ?
O6 C31 Mo C28 -124(3) . . . . ?
O6 C31 Mo P 146(3) . . . . ?
O3 C28 Mo C27 14(11) . . . . ?
O3 C28 Mo C30 170(100) . . . . ?
O3 C28 Mo C29 -74(11) . . . . ?
O3 C28 Mo C31 100(11) . . . . ?
O3 C28 Mo P -170(11) . . . . ?
O1 P Mo C27 -56.4(16) . . . . ?
C1 P Mo C27 2.4(17) . . . . ?
C8 P Mo C27 155.7(16) . . . . ?
O1 P Mo C30 50.07(17) . . . . ?
C1 P Mo C30 108.90(19) . . . . ?
C8 P Mo C30 -97.82(19) . . . . ?
O1 P Mo C29 138.75(17) . . . . ?
C1 P Mo C29 -162.4(2) . . . . ?
C8 P Mo C29 -9.1(2) . . . . ?
O1 P Mo C31 -37.13(17) . . . . ?
C1 P Mo C31 21.7(2) . . . . ?
C8 P Mo C31 174.98(19) . . . . ?
O1 P Mo C28 -129.89(16) . . . . ?
C1 P Mo C28 -71.06(19) . . . . ?
C8 P Mo C28 82.22(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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_2546
_database_code_depnum_ccdc_archive 'CCDC 1423353'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C55 H34 Mo2 O12 P2, C4 H10 O'
_chemical_formula_sum            'C59 H44 Mo2 O13 P2'
_chemical_formula_weight         1214.76

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'
Mo Mo -1.6832 0.6857 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.286(8)
_cell_length_b                   18.409(9)
_cell_length_c                   23.093(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.99(4)
_cell_angle_gamma                90.00
_cell_volume                     5481(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    166
_cell_measurement_theta_min      3.53
_cell_measurement_theta_max      25.34

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2464
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_type   Integration
_exptl_absorpt_correction_T_min  0.8183
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_process_details   'STOE Xred'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            51069
_diffrn_reflns_av_R_equivalents  0.1524
_diffrn_reflns_av_sigmaI/netI    0.1594
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         28.00
_reflns_number_total             13213
_reflns_number_gt                7302
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0237P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13213
_refine_ls_number_parameters     687
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0858
_refine_ls_goodness_of_fit_ref   0.789
_refine_ls_restrained_S_all      0.788
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6636(3) 0.2555(2) 0.55502(15) 0.0154(8) Uani 1 1 d . . .
C2 C 0.5919(3) 0.1918(2) 0.55834(16) 0.0145(8) Uani 1 1 d . . .
C3 C 0.6454(3) 0.1264(2) 0.56147(16) 0.0159(8) Uani 1 1 d . . .
C4 C 0.6406(3) 0.3271(2) 0.58035(17) 0.0177(8) Uani 1 1 d . . .
C5 C 0.5486(3) 0.3635(2) 0.55565(19) 0.0237(9) Uani 1 1 d . . .
H5A H 0.4998 0.3421 0.5232 0.028 Uiso 1 1 calc R . .
C6 C 0.5260(3) 0.4308(3) 0.5773(2) 0.0273(10) Uani 1 1 d . . .
H6A H 0.4622 0.4544 0.5601 0.033 Uiso 1 1 calc R . .
C7 C 0.5972(4) 0.4626(3) 0.6239(2) 0.0356(12) Uani 1 1 d . . .
H7A H 0.5834 0.5088 0.6387 0.043 Uiso 1 1 calc R . .
C8 C 0.6888(4) 0.4266(3) 0.6490(2) 0.0335(11) Uani 1 1 d . . .
H8A H 0.7378 0.4484 0.6811 0.040 Uiso 1 1 calc R . .
C9 C 0.7102(3) 0.3597(3) 0.62807(19) 0.0255(10) Uani 1 1 d . . .
H9A H 0.7730 0.3356 0.6464 0.031 Uiso 1 1 calc R . .
C10 C 0.6832(3) 0.2605(2) 0.48934(15) 0.0164(8) Uani 1 1 d . . .
H10A H 0.7353 0.3000 0.4903 0.020 Uiso 1 1 calc R . .
C11 C 0.7365(3) 0.1884(2) 0.48000(16) 0.0155(8) Uani 1 1 d . . .
H11A H 0.8001 0.1987 0.4654 0.019 Uiso 1 1 calc R . .
C12 C 0.6708(3) 0.1337(2) 0.44011(16) 0.0192(9) Uani 1 1 d . . .
H12A H 0.7015 0.0884 0.4347 0.023 Uiso 1 1 calc R . .
C13 C 0.5725(3) 0.1443(2) 0.41180(17) 0.0161(8) Uani 1 1 d . . .
H13A H 0.5349 0.1050 0.3902 0.019 Uiso 1 1 calc R . .
C14 C 0.5180(3) 0.2157(2) 0.41242(16) 0.0161(8) Uani 1 1 d . . .
H14A H 0.4698 0.2095 0.4393 0.019 Uiso 1 1 calc R . .
C15 C 0.5921(3) 0.2772(2) 0.43838(16) 0.0156(8) Uani 1 1 d . . .
C16 C 0.4875(3) 0.1919(2) 0.55682(16) 0.0184(9) Uani 1 1 d . . .
H16A H 0.4506 0.2363 0.5556 0.022 Uiso 1 1 calc R . .
C17 C 0.4368(3) 0.1253(3) 0.55716(18) 0.0229(9) Uani 1 1 d . . .
H17A H 0.3647 0.1246 0.5557 0.027 Uiso 1 1 calc R . .
C18 C 0.4902(3) 0.0606(3) 0.55954(17) 0.0229(9) Uani 1 1 d . . .
H18A H 0.4543 0.0159 0.5595 0.028 Uiso 1 1 calc R . .
C19 C 0.5950(3) 0.0600(2) 0.56204(16) 0.0204(9) Uani 1 1 d . . .
H19A H 0.6319 0.0155 0.5641 0.024 Uiso 1 1 calc R . .
C20 C 1.0536(4) 0.0076(3) 0.6139(2) 0.0370(12) Uani 1 1 d . . .
C21 C 0.8634(4) 0.0226(3) 0.6532(2) 0.0286(11) Uani 1 1 d . . .
C22 C 0.8536(3) 0.0005(3) 0.52666(19) 0.0236(10) Uani 1 1 d . . .
C23 C 0.9882(3) 0.1237(3) 0.5289(2) 0.0289(11) Uani 1 1 d . . .
C24 C 0.9878(4) 0.1479(3) 0.6558(2) 0.0323(11) Uani 1 1 d . . .
C25 C 0.5768(3) 0.3380(2) 0.40497(18) 0.0165(8) Uani 1 1 d . . .
C26 C 0.6400(3) 0.4052(2) 0.40922(18) 0.0184(9) Uani 1 1 d . . .
C27 C 0.6938(3) 0.4349(2) 0.46386(18) 0.0212(9) Uani 1 1 d . . .
H27A H 0.6846 0.4153 0.5003 0.025 Uiso 1 1 calc R . .
C28 C 0.7599(4) 0.4928(2) 0.4647(2) 0.0268(10) Uani 1 1 d . . .
H28A H 0.7978 0.5117 0.5018 0.032 Uiso 1 1 calc R . .
C29 C 0.7716(3) 0.5233(3) 0.4126(2) 0.0280(10) Uani 1 1 d . . .
H29A H 0.8179 0.5629 0.4138 0.034 Uiso 1 1 calc R . .
C30 C 0.7160(3) 0.4963(3) 0.3580(2) 0.0269(10) Uani 1 1 d . . .
H30A H 0.7228 0.5182 0.3219 0.032 Uiso 1 1 calc R . .
C31 C 0.6505(3) 0.4373(2) 0.35628(18) 0.0209(9) Uani 1 1 d . . .
H31A H 0.6128 0.4187 0.3190 0.025 Uiso 1 1 calc R . .
C32 C 0.4881(3) 0.2226(2) 0.27131(16) 0.0148(8) Uani 1 1 d . . .
C33 C 0.4979(3) 0.1395(2) 0.27719(16) 0.0169(8) Uani 1 1 d . . .
C34 C 0.5877(3) 0.1027(2) 0.27477(18) 0.0210(9) Uani 1 1 d . . .
H34A H 0.6448 0.1290 0.2673 0.025 Uiso 1 1 calc R . .
C35 C 0.5959(4) 0.0276(2) 0.28313(19) 0.0255(10) Uani 1 1 d . . .
H35A H 0.6582 0.0033 0.2815 0.031 Uiso 1 1 calc R . .
C36 C 0.5131(4) -0.0114(3) 0.29389(18) 0.0267(10) Uani 1 1 d . . .
H36A H 0.5191 -0.0623 0.3009 0.032 Uiso 1 1 calc R . .
C37 C 0.4221(3) 0.0240(2) 0.29429(17) 0.0231(10) Uani 1 1 d . . .
H37A H 0.3647 -0.0026 0.3010 0.028 Uiso 1 1 calc R . .
C38 C 0.4139(3) 0.0988(2) 0.28481(16) 0.0178(9) Uani 1 1 d . . .
H38A H 0.3498 0.1224 0.2835 0.021 Uiso 1 1 calc R . .
C39 C 0.5904(3) 0.2602(2) 0.26999(16) 0.0165(8) Uani 1 1 d . . .
C40 C 0.6777(3) 0.2514(2) 0.31796(16) 0.0180(8) Uani 1 1 d . . .
H40A H 0.6719 0.2229 0.3513 0.022 Uiso 1 1 calc R . .
C41 C 0.7724(3) 0.2833(3) 0.31773(19) 0.0250(10) Uani 1 1 d . . .
H41A H 0.8302 0.2773 0.3508 0.030 Uiso 1 1 calc R . .
C42 C 0.7817(3) 0.3238(3) 0.26893(19) 0.0251(10) Uani 1 1 d . . .
H42A H 0.8461 0.3461 0.2686 0.030 Uiso 1 1 calc R . .
C43 C 0.6976(3) 0.3320(3) 0.22061(19) 0.0235(10) Uani 1 1 d . . .
H43A H 0.7046 0.3593 0.1869 0.028 Uiso 1 1 calc R . .
C44 C 0.6029(3) 0.3004(2) 0.22134(17) 0.0189(9) Uani 1 1 d . . .
H44A H 0.5456 0.3065 0.1879 0.023 Uiso 1 1 calc R . .
C45 C 0.4029(3) 0.2432(2) 0.21552(16) 0.0172(8) Uani 1 1 d . . .
C46 C 0.3586(3) 0.3127(2) 0.21025(17) 0.0199(9) Uani 1 1 d . . .
H46A H 0.3807 0.3470 0.2415 0.024 Uiso 1 1 calc R . .
C47 C 0.2830(3) 0.3321(3) 0.15999(19) 0.0251(10) Uani 1 1 d . . .
H47A H 0.2533 0.3793 0.1572 0.030 Uiso 1 1 calc R . .
C48 C 0.2502(3) 0.2825(3) 0.11330(19) 0.0256(10) Uani 1 1 d . . .
H48A H 0.1968 0.2953 0.0794 0.031 Uiso 1 1 calc R . .
C49 C 0.2958(3) 0.2154(3) 0.11710(19) 0.0255(10) Uani 1 1 d . . .
H49A H 0.2757 0.1822 0.0849 0.031 Uiso 1 1 calc R . .
C50 C 0.3716(3) 0.1951(2) 0.16783(17) 0.0211(9) Uani 1 1 d . . .
H50A H 0.4020 0.1481 0.1699 0.025 Uiso 1 1 calc R . .
C51 C 0.1066(3) 0.2665(3) 0.3537(2) 0.0362(12) Uani 1 1 d . . .
C52 C 0.2697(3) 0.1646(3) 0.3874(2) 0.0244(10) Uani 1 1 d . . .
C53 C 0.1910(3) 0.2083(3) 0.26256(19) 0.0237(9) Uani 1 1 d U . .
C54 C 0.2267(3) 0.3602(3) 0.2987(2) 0.0268(10) Uani 1 1 d . . .
C55 C 0.2949(3) 0.3158(3) 0.4211(2) 0.0287(10) Uani 1 1 d . . .
C56 C 0.9769(7) -0.0350(5) 0.1447(4) 0.101(3) Uani 1 1 d U . .
H56C H 0.9858 -0.0466 0.1871 0.121 Uiso 1 1 calc R . .
H56B H 1.0328 -0.0575 0.1301 0.121 Uiso 1 1 calc R . .
H56A H 0.9098 -0.0537 0.1220 0.121 Uiso 1 1 calc R . .
C57 C 0.9801(6) 0.0449(5) 0.1372(3) 0.069(2) Uani 1 1 d U . .
H57A H 0.9210 0.0675 0.1497 0.083 Uiso 1 1 calc R . .
H57B H 1.0451 0.0644 0.1630 0.083 Uiso 1 1 calc R . .
C59 C 0.9756(6) 0.1381(4) 0.0646(3) 0.070(2) Uani 1 1 d U . .
H59A H 1.0369 0.1612 0.0912 0.084 Uiso 1 1 calc R . .
H59B H 0.9126 0.1612 0.0721 0.084 Uiso 1 1 calc R . .
C60 C 0.9785(5) 0.1495(5) 0.0024(3) 0.075(2) Uani 1 1 d U . .
H60C H 0.9954 0.2003 -0.0034 0.090 Uiso 1 1 calc R . .
H60B H 0.9106 0.1378 -0.0237 0.090 Uiso 1 1 calc R . .
H60A H 1.0315 0.1179 -0.0074 0.090 Uiso 1 1 calc R . .
Mo1 Mo 0.92591(3) 0.07260(2) 0.590710(17) 0.02108(9) Uani 1 1 d . . .
Mo2 Mo 0.25002(3) 0.26134(2) 0.342339(16) 0.01767(8) Uani 1 1 d U . .
O1 O 0.76568(19) 0.22984(15) 0.58858(11) 0.0175(6) Uani 1 1 d . . .
O2 O 1.1241(3) -0.0287(2) 0.6270(2) 0.0590(12) Uani 1 1 d . . .
O3 O 0.8325(3) -0.0058(2) 0.68941(16) 0.0443(9) Uani 1 1 d . . .
O4 O 0.8112(3) -0.03797(19) 0.49008(15) 0.0330(8) Uani 1 1 d . . .
O5 O 1.0202(3) 0.1529(2) 0.49363(17) 0.0422(9) Uani 1 1 d . . .
O6 O 1.0171(3) 0.1898(3) 0.69253(18) 0.0585(12) Uani 1 1 d . . .
O7 O 0.4942(2) 0.33647(15) 0.35425(11) 0.0155(6) Uani 1 1 d . . .
O8 O 0.0251(3) 0.2679(3) 0.36264(19) 0.0592(12) Uani 1 1 d . . .
O9 O 0.2796(3) 0.1113(2) 0.41337(16) 0.0424(9) Uani 1 1 d . . .
O10 O 0.1545(3) 0.1781(2) 0.21952(15) 0.0368(8) Uani 1 1 d . . .
O11 O 0.2108(3) 0.41435(18) 0.27523(15) 0.0356(8) Uani 1 1 d . . .
O12 O 0.3130(3) 0.3473(2) 0.46520(16) 0.0505(11) Uani 1 1 d . . .
O13 O 0.9749(3) 0.0625(3) 0.0776(2) 0.0616(12) Uani 1 1 d U . .
P1 P 0.77510(8) 0.15007(6) 0.55818(5) 0.0170(2) Uani 1 1 d . . .
P2 P 0.43911(7) 0.25571(6) 0.34036(4) 0.0143(2) Uani 1 1 d . . .


_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
C1 O1 1.468(4) . ?
C1 C4 1.502(6) . ?
C1 C2 1.525(6) . ?
C1 C10 1.602(5) . ?
C2 C16 1.379(6) . ?
C2 C3 1.392(6) . ?
C3 C19 1.394(6) . ?
C3 P1 1.797(4) . ?
C4 C5 1.390(6) . ?
C4 C9 1.392(6) . ?
C5 C6 1.395(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.380(7) . ?
C6 H6A 0.9500 . ?
C7 C8 1.384(7) . ?
C7 H7A 0.9500 . ?
C8 C9 1.377(7) . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?
C10 C15 1.502(5) . ?
C10 C11 1.545(6) . ?
C10 H10A 1.0000 . ?
C11 C12 1.494(6) . ?
C11 P1 1.890(4) . ?
C11 H11A 1.0000 . ?
C12 C13 1.326(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.502(5) . ?
C13 H13A 0.9500 . ?
C14 C15 1.526(5) . ?
C14 P2 1.889(4) . ?
C14 H14A 1.0000 . ?
C15 C25 1.347(5) . ?
C16 C17 1.400(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.380(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.380(6) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 O2 1.132(6) . ?
C20 Mo1 2.038(5) . ?
C21 O3 1.143(6) . ?
C21 Mo1 2.049(5) . ?
C22 O4 1.141(5) . ?
C22 Mo1 2.046(5) . ?
C23 O5 1.140(6) . ?
C23 Mo1 2.045(5) . ?
C24 O6 1.142(6) . ?
C24 Mo1 2.064(5) . ?
C25 O7 1.399(5) . ?
C25 C26 1.484(6) . ?
C26 C31 1.395(6) . ?
C26 C27 1.403(5) . ?
C27 C28 1.378(6) . ?
C27 H27A 0.9500 . ?
C28 C29 1.370(7) . ?
C28 H28A 0.9500 . ?
C29 C30 1.390(6) . ?
C29 H29A 0.9500 . ?
C30 C31 1.385(6) . ?
C30 H30A 0.9500 . ?
C31 H31A 0.9500 . ?
C32 C39 1.531(5) . ?
C32 C33 1.539(5) . ?
C32 C45 1.543(5) . ?
C32 P2 1.960(4) . ?
C33 C34 1.385(6) . ?
C33 C38 1.390(6) . ?
C34 C35 1.396(6) . ?
C34 H34A 0.9500 . ?
C35 C36 1.387(7) . ?
C35 H35A 0.9500 . ?
C36 C37 1.375(6) . ?
C36 H36A 0.9500 . ?
C37 C38 1.396(6) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
C39 C44 1.389(6) . ?
C39 C40 1.407(5) . ?
C40 C41 1.389(6) . ?
C40 H40A 0.9500 . ?
C41 C42 1.382(6) . ?
C41 H41A 0.9500 . ?
C42 C43 1.383(6) . ?
C42 H42A 0.9500 . ?
C43 C44 1.391(6) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C50 1.397(6) . ?
C45 C46 1.400(6) . ?
C46 C47 1.385(6) . ?
C46 H46A 0.9500 . ?
C47 C48 1.399(6) . ?
C47 H47A 0.9500 . ?
C48 C49 1.370(7) . ?
C48 H48A 0.9500 . ?
C49 C50 1.399(6) . ?
C49 H49A 0.9500 . ?
C50 H50A 0.9500 . ?
C51 O8 1.150(5) . ?
C51 Mo2 1.988(5) . ?
C52 O9 1.140(5) . ?
C52 Mo2 2.047(5) . ?
C53 O10 1.140(5) . ?
C53 Mo2 2.065(5) . ?
C54 O11 1.130(6) . ?
C54 Mo2 2.067(5) . ?
C55 O12 1.145(5) . ?
C55 Mo2 2.036(5) . ?
C56 C57 1.484(12) . ?
C56 H56C 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56A 0.9800 . ?
C57 O13 1.400(8) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C59 O13 1.424(8) . ?
C59 C60 1.461(10) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60C 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60A 0.9800 . ?
Mo1 P1 2.4258(15) . ?
Mo2 P2 2.5259(18) . ?
O1 P1 1.646(3) . ?
O7 P2 1.654(3) . ?

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 C1 C4 109.0(3) . . ?
O1 C1 C2 103.6(3) . . ?
C4 C1 C2 117.8(3) . . ?
O1 C1 C10 100.2(3) . . ?
C4 C1 C10 114.4(3) . . ?
C2 C1 C10 109.8(3) . . ?
C16 C2 C3 120.0(4) . . ?
C16 C2 C1 129.4(4) . . ?
C3 C2 C1 110.5(3) . . ?
C2 C3 C19 121.2(4) . . ?
C2 C3 P1 105.7(3) . . ?
C19 C3 P1 132.9(3) . . ?
C5 C4 C9 117.8(4) . . ?
C5 C4 C1 120.3(4) . . ?
C9 C4 C1 121.9(4) . . ?
C4 C5 C6 121.7(4) . . ?
C4 C5 H5A 119.2 . . ?
C6 C5 H5A 119.2 . . ?
C7 C6 C5 119.3(4) . . ?
C7 C6 H6A 120.3 . . ?
C5 C6 H6A 120.3 . . ?
C6 C7 C8 119.4(4) . . ?
C6 C7 H7A 120.3 . . ?
C8 C7 H7A 120.3 . . ?
C9 C8 C7 121.1(4) . . ?
C9 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
C8 C9 C4 120.7(4) . . ?
C8 C9 H9A 119.7 . . ?
C4 C9 H9A 119.7 . . ?
C15 C10 C11 112.1(3) . . ?
C15 C10 C1 117.9(3) . . ?
C11 C10 C1 105.5(3) . . ?
C15 C10 H10A 106.9 . . ?
C11 C10 H10A 106.9 . . ?
C1 C10 H10A 106.9 . . ?
C12 C11 C10 116.5(3) . . ?
C12 C11 P1 108.7(3) . . ?
C10 C11 P1 102.4(2) . . ?
C12 C11 H11A 109.6 . . ?
C10 C11 H11A 109.6 . . ?
P1 C11 H11A 109.6 . . ?
C13 C12 C11 124.3(4) . . ?
C13 C12 H12A 117.8 . . ?
C11 C12 H12A 117.8 . . ?
C12 C13 C14 122.9(4) . . ?
C12 C13 H13A 118.5 . . ?
C14 C13 H13A 118.5 . . ?
C13 C14 C15 112.7(3) . . ?
C13 C14 P2 119.9(3) . . ?
C15 C14 P2 103.0(3) . . ?
C13 C14 H14A 106.8 . . ?
C15 C14 H14A 106.8 . . ?
P2 C14 H14A 106.8 . . ?
C25 C15 C10 126.9(4) . . ?
C25 C15 C14 113.5(3) . . ?
C10 C15 C14 118.5(3) . . ?
C2 C16 C17 118.8(4) . . ?
C2 C16 H16A 120.6 . . ?
C17 C16 H16A 120.6 . . ?
C18 C17 C16 120.9(4) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C19 C18 C17 120.7(4) . . ?
C19 C18 H18A 119.6 . . ?
C17 C18 H18A 119.6 . . ?
C18 C19 C3 118.4(4) . . ?
C18 C19 H19A 120.8 . . ?
C3 C19 H19A 120.8 . . ?
O2 C20 Mo1 179.5(6) . . ?
O3 C21 Mo1 177.2(4) . . ?
O4 C22 Mo1 177.8(4) . . ?
O5 C23 Mo1 178.1(4) . . ?
O6 C24 Mo1 176.4(5) . . ?
C15 C25 O7 116.2(4) . . ?
C15 C25 C26 130.5(4) . . ?
O7 C25 C26 112.9(3) . . ?
C31 C26 C27 119.0(4) . . ?
C31 C26 C25 118.1(4) . . ?
C27 C26 C25 122.8(4) . . ?
C28 C27 C26 119.9(4) . . ?
C28 C27 H27A 120.0 . . ?
C26 C27 H27A 120.0 . . ?
C29 C28 C27 120.8(4) . . ?
C29 C28 H28A 119.6 . . ?
C27 C28 H28A 119.6 . . ?
C28 C29 C30 120.0(4) . . ?
C28 C29 H29A 120.0 . . ?
C30 C29 H29A 120.0 . . ?
C31 C30 C29 119.9(4) . . ?
C31 C30 H30A 120.0 . . ?
C29 C30 H30A 120.0 . . ?
C30 C31 C26 120.2(4) . . ?
C30 C31 H31A 119.9 . . ?
C26 C31 H31A 119.9 . . ?
C39 C32 C33 113.2(3) . . ?
C39 C32 C45 110.4(3) . . ?
C33 C32 C45 110.3(3) . . ?
C39 C32 P2 110.3(3) . . ?
C33 C32 P2 106.0(3) . . ?
C45 C32 P2 106.4(3) . . ?
C34 C33 C38 117.9(4) . . ?
C34 C33 C32 122.6(4) . . ?
C38 C33 C32 119.6(4) . . ?
C33 C34 C35 121.2(4) . . ?
C33 C34 H34A 119.4 . . ?
C35 C34 H34A 119.4 . . ?
C36 C35 C34 119.9(4) . . ?
C36 C35 H35A 120.0 . . ?
C34 C35 H35A 120.0 . . ?
C37 C36 C35 119.5(4) . . ?
C37 C36 H36A 120.2 . . ?
C35 C36 H36A 120.2 . . ?
C36 C37 C38 120.2(4) . . ?
C36 C37 H37A 119.9 . . ?
C38 C37 H37A 119.9 . . ?
C33 C38 C37 121.1(4) . . ?
C33 C38 H38A 119.4 . . ?
C37 C38 H38A 119.4 . . ?
C44 C39 C40 117.5(4) . . ?
C44 C39 C32 122.5(3) . . ?
C40 C39 C32 120.0(3) . . ?
C41 C40 C39 121.6(4) . . ?
C41 C40 H40A 119.2 . . ?
C39 C40 H40A 119.2 . . ?
C42 C41 C40 119.4(4) . . ?
C42 C41 H41A 120.3 . . ?
C40 C41 H41A 120.3 . . ?
C41 C42 C43 120.2(4) . . ?
C41 C42 H42A 119.9 . . ?
C43 C42 H42A 119.9 . . ?
C42 C43 C44 120.1(4) . . ?
C42 C43 H43A 120.0 . . ?
C44 C43 H43A 120.0 . . ?
C39 C44 C43 121.2(4) . . ?
C39 C44 H44A 119.4 . . ?
C43 C44 H44A 119.4 . . ?
C50 C45 C46 118.2(4) . . ?
C50 C45 C32 121.4(4) . . ?
C46 C45 C32 120.3(3) . . ?
C47 C46 C45 120.8(4) . . ?
C47 C46 H46A 119.6 . . ?
C45 C46 H46A 119.6 . . ?
C46 C47 C48 120.4(4) . . ?
C46 C47 H47A 119.8 . . ?
C48 C47 H47A 119.8 . . ?
C49 C48 C47 119.2(4) . . ?
C49 C48 H48A 120.4 . . ?
C47 C48 H48A 120.4 . . ?
C48 C49 C50 120.9(4) . . ?
C48 C49 H49A 119.6 . . ?
C50 C49 H49A 119.6 . . ?
C45 C50 C49 120.5(4) . . ?
C45 C50 H50A 119.8 . . ?
C49 C50 H50A 119.8 . . ?
O8 C51 Mo2 176.9(5) . . ?
O9 C52 Mo2 178.5(4) . . ?
O10 C53 Mo2 176.7(4) . . ?
O11 C54 Mo2 177.7(4) . . ?
O12 C55 Mo2 175.2(4) . . ?
C57 C56 H56C 109.5 . . ?
C57 C56 H56B 109.5 . . ?
H56C C56 H56B 109.5 . . ?
C57 C56 H56A 109.5 . . ?
H56C C56 H56A 109.5 . . ?
H56B C56 H56A 109.5 . . ?
O13 C57 C56 110.4(7) . . ?
O13 C57 H57A 109.6 . . ?
C56 C57 H57A 109.6 . . ?
O13 C57 H57B 109.6 . . ?
C56 C57 H57B 109.6 . . ?
H57A C57 H57B 108.1 . . ?
O13 C59 C60 110.6(7) . . ?
O13 C59 H59A 109.5 . . ?
C60 C59 H59A 109.5 . . ?
O13 C59 H59B 109.5 . . ?
C60 C59 H59B 109.5 . . ?
H59A C59 H59B 108.1 . . ?
C59 C60 H60C 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60C C60 H60B 109.5 . . ?
C59 C60 H60A 109.5 . . ?
H60C C60 H60A 109.5 . . ?
H60B C60 H60A 109.5 . . ?
C20 Mo1 C23 90.1(2) . . ?
C20 Mo1 C22 91.4(2) . . ?
C23 Mo1 C22 89.57(19) . . ?
C20 Mo1 C21 90.3(2) . . ?
C23 Mo1 C21 179.3(2) . . ?
C22 Mo1 C21 91.02(18) . . ?
C20 Mo1 C24 92.5(2) . . ?
C23 Mo1 C24 92.4(2) . . ?
C22 Mo1 C24 175.62(18) . . ?
C21 Mo1 C24 87.0(2) . . ?
C20 Mo1 P1 177.19(16) . . ?
C23 Mo1 P1 87.51(13) . . ?
C22 Mo1 P1 87.08(13) . . ?
C21 Mo1 P1 92.14(14) . . ?
C24 Mo1 P1 89.11(14) . . ?
C51 Mo2 C55 86.7(2) . . ?
C51 Mo2 C52 89.1(2) . . ?
C55 Mo2 C52 90.0(2) . . ?
C51 Mo2 C53 88.33(19) . . ?
C55 Mo2 C53 174.91(18) . . ?
C52 Mo2 C53 90.94(18) . . ?
C51 Mo2 C54 89.2(2) . . ?
C55 Mo2 C54 88.7(2) . . ?
C52 Mo2 C54 177.96(19) . . ?
C53 Mo2 C54 90.13(18) . . ?
C51 Mo2 P2 173.66(14) . . ?
C55 Mo2 P2 87.61(14) . . ?
C52 Mo2 P2 88.17(13) . . ?
C53 Mo2 P2 97.42(13) . . ?
C54 Mo2 P2 93.42(13) . . ?
C1 O1 P1 102.6(2) . . ?
C25 O7 P2 113.7(2) . . ?
C57 O13 C59 115.6(6) . . ?
O1 P1 C3 91.49(17) . . ?
O1 P1 C11 92.50(16) . . ?
C3 P1 C11 95.13(18) . . ?
O1 P1 Mo1 122.33(10) . . ?
C3 P1 Mo1 124.95(14) . . ?
C11 P1 Mo1 121.89(13) . . ?
O7 P2 C14 93.15(16) . . ?
O7 P2 C32 102.64(16) . . ?
C14 P2 C32 111.90(17) . . ?
O7 P2 Mo2 110.79(11) . . ?
C14 P2 Mo2 110.02(13) . . ?
C32 P2 Mo2 123.72(12) . . ?

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
O1 C1 C2 C16 151.5(4) . . . . ?
C4 C1 C2 C16 31.1(5) . . . . ?
C10 C1 C2 C16 -102.2(4) . . . . ?
O1 C1 C2 C3 -30.6(4) . . . . ?
C4 C1 C2 C3 -151.0(3) . . . . ?
C10 C1 C2 C3 75.7(4) . . . . ?
C16 C2 C3 C19 1.2(6) . . . . ?
C1 C2 C3 C19 -177.0(3) . . . . ?
C16 C2 C3 P1 176.8(3) . . . . ?
C1 C2 C3 P1 -1.4(4) . . . . ?
O1 C1 C4 C5 179.1(4) . . . . ?
C2 C1 C4 C5 -63.4(5) . . . . ?
C10 C1 C4 C5 67.8(5) . . . . ?
O1 C1 C4 C9 0.2(5) . . . . ?
C2 C1 C4 C9 117.7(4) . . . . ?
C10 C1 C4 C9 -111.0(4) . . . . ?
C9 C4 C5 C6 0.4(7) . . . . ?
C1 C4 C5 C6 -178.6(4) . . . . ?
C4 C5 C6 C7 0.9(7) . . . . ?
C5 C6 C7 C8 -1.1(7) . . . . ?
C6 C7 C8 C9 0.2(8) . . . . ?
C7 C8 C9 C4 1.1(8) . . . . ?
C5 C4 C9 C8 -1.3(7) . . . . ?
C1 C4 C9 C8 177.6(4) . . . . ?
O1 C1 C10 C15 173.1(3) . . . . ?
C4 C1 C10 C15 -70.4(4) . . . . ?
C2 C1 C10 C15 64.6(5) . . . . ?
O1 C1 C10 C11 47.0(3) . . . . ?
C4 C1 C10 C11 163.5(3) . . . . ?
C2 C1 C10 C11 -61.5(4) . . . . ?
C15 C10 C11 C12 -24.8(5) . . . . ?
C1 C10 C11 C12 104.9(4) . . . . ?
C15 C10 C11 P1 -143.3(3) . . . . ?
C1 C10 C11 P1 -13.6(3) . . . . ?
C10 C11 C12 C13 1.8(6) . . . . ?
P1 C11 C12 C13 116.8(4) . . . . ?
C11 C12 C13 C14 5.5(7) . . . . ?
C12 C13 C14 C15 11.0(6) . . . . ?
C12 C13 C14 P2 132.4(4) . . . . ?
C11 C10 C15 C25 -124.5(4) . . . . ?
C1 C10 C15 C25 112.7(5) . . . . ?
C11 C10 C15 C14 42.6(5) . . . . ?
C1 C10 C15 C14 -80.2(5) . . . . ?
C13 C14 C15 C25 132.7(4) . . . . ?
P2 C14 C15 C25 2.1(4) . . . . ?
C13 C14 C15 C10 -36.1(5) . . . . ?
P2 C14 C15 C10 -166.7(3) . . . . ?
C3 C2 C16 C17 -1.4(6) . . . . ?
C1 C2 C16 C17 176.3(4) . . . . ?
C2 C16 C17 C18 0.6(6) . . . . ?
C16 C17 C18 C19 0.4(6) . . . . ?
C17 C18 C19 C3 -0.7(6) . . . . ?
C2 C3 C19 C18 -0.1(6) . . . . ?
P1 C3 C19 C18 -174.3(3) . . . . ?
C10 C15 C25 O7 170.5(3) . . . . ?
C14 C15 C25 O7 2.8(5) . . . . ?
C10 C15 C25 C26 -2.4(7) . . . . ?
C14 C15 C25 C26 -170.1(4) . . . . ?
C15 C25 C26 C31 140.2(5) . . . . ?
O7 C25 C26 C31 -32.8(5) . . . . ?
C15 C25 C26 C27 -36.1(7) . . . . ?
O7 C25 C26 C27 150.9(4) . . . . ?
C31 C26 C27 C28 -3.3(6) . . . . ?
C25 C26 C27 C28 173.0(4) . . . . ?
C26 C27 C28 C29 2.0(7) . . . . ?
C27 C28 C29 C30 0.4(7) . . . . ?
C28 C29 C30 C31 -1.6(7) . . . . ?
C29 C30 C31 C26 0.3(7) . . . . ?
C27 C26 C31 C30 2.1(6) . . . . ?
C25 C26 C31 C30 -174.3(4) . . . . ?
C39 C32 C33 C34 -6.7(5) . . . . ?
C45 C32 C33 C34 117.5(4) . . . . ?
P2 C32 C33 C34 -127.7(3) . . . . ?
C39 C32 C33 C38 173.8(3) . . . . ?
C45 C32 C33 C38 -62.0(4) . . . . ?
P2 C32 C33 C38 52.8(4) . . . . ?
C38 C33 C34 C35 -3.6(6) . . . . ?
C32 C33 C34 C35 176.9(4) . . . . ?
C33 C34 C35 C36 0.2(7) . . . . ?
C34 C35 C36 C37 2.1(6) . . . . ?
C35 C36 C37 C38 -0.9(6) . . . . ?
C34 C33 C38 C37 4.8(6) . . . . ?
C32 C33 C38 C37 -175.7(3) . . . . ?
C36 C37 C38 C33 -2.6(6) . . . . ?
C33 C32 C39 C44 118.2(4) . . . . ?
C45 C32 C39 C44 -6.1(5) . . . . ?
P2 C32 C39 C44 -123.3(4) . . . . ?
C33 C32 C39 C40 -58.4(5) . . . . ?
C45 C32 C39 C40 177.3(4) . . . . ?
P2 C32 C39 C40 60.1(4) . . . . ?
C44 C39 C40 C41 1.8(6) . . . . ?
C32 C39 C40 C41 178.5(4) . . . . ?
C39 C40 C41 C42 -1.0(7) . . . . ?
C40 C41 C42 C43 -0.4(7) . . . . ?
C41 C42 C43 C44 0.9(7) . . . . ?
C40 C39 C44 C43 -1.3(6) . . . . ?
C32 C39 C44 C43 -177.9(4) . . . . ?
C42 C43 C44 C39 -0.1(7) . . . . ?
C39 C32 C45 C50 103.4(4) . . . . ?
C33 C32 C45 C50 -22.5(5) . . . . ?
P2 C32 C45 C50 -136.9(3) . . . . ?
C39 C32 C45 C46 -73.2(4) . . . . ?
C33 C32 C45 C46 160.9(4) . . . . ?
P2 C32 C45 C46 46.5(4) . . . . ?
C50 C45 C46 C47 2.4(6) . . . . ?
C32 C45 C46 C47 179.1(4) . . . . ?
C45 C46 C47 C48 -0.5(6) . . . . ?
C46 C47 C48 C49 -1.9(6) . . . . ?
C47 C48 C49 C50 2.4(7) . . . . ?
C46 C45 C50 C49 -1.9(6) . . . . ?
C32 C45 C50 C49 -178.6(4) . . . . ?
C48 C49 C50 C45 -0.5(6) . . . . ?
O2 C20 Mo1 C23 -176(100) . . . . ?
O2 C20 Mo1 C22 -87(81) . . . . ?
O2 C20 Mo1 C21 4(81) . . . . ?
O2 C20 Mo1 C24 91(81) . . . . ?
O2 C20 Mo1 P1 -144(79) . . . . ?
O5 C23 Mo1 C20 160(14) . . . . ?
O5 C23 Mo1 C22 69(14) . . . . ?
O5 C23 Mo1 C21 -78(22) . . . . ?
O5 C23 Mo1 C24 -107(14) . . . . ?
O5 C23 Mo1 P1 -18(14) . . . . ?
O4 C22 Mo1 C20 -160(11) . . . . ?
O4 C22 Mo1 C23 -70(11) . . . . ?
O4 C22 Mo1 C21 110(11) . . . . ?
O4 C22 Mo1 C24 47(12) . . . . ?
O4 C22 Mo1 P1 18(11) . . . . ?
O3 C21 Mo1 C20 30(9) . . . . ?
O3 C21 Mo1 C23 -91(18) . . . . ?
O3 C21 Mo1 C22 122(9) . . . . ?
O3 C21 Mo1 C24 -62(9) . . . . ?
O3 C21 Mo1 P1 -151(9) . . . . ?
O6 C24 Mo1 C20 -136(7) . . . . ?
O6 C24 Mo1 C23 134(7) . . . . ?
O6 C24 Mo1 C22 17(9) . . . . ?
O6 C24 Mo1 C21 -45(7) . . . . ?
O6 C24 Mo1 P1 47(7) . . . . ?
O8 C51 Mo2 C55 -58(10) . . . . ?
O8 C51 Mo2 C52 32(10) . . . . ?
O8 C51 Mo2 C53 123(10) . . . . ?
O8 C51 Mo2 C54 -147(10) . . . . ?
O8 C51 Mo2 P2 -32(11) . . . . ?
O12 C55 Mo2 C51 -10(6) . . . . ?
O12 C55 Mo2 C52 -99(6) . . . . ?
O12 C55 Mo2 C53 2(7) . . . . ?
O12 C55 Mo2 C54 80(6) . . . . ?
O12 C55 Mo2 P2 173(6) . . . . ?
O9 C52 Mo2 C51 -40(18) . . . . ?
O9 C52 Mo2 C55 46(18) . . . . ?
O9 C52 Mo2 C53 -129(18) . . . . ?
O9 C52 Mo2 C54 -7(21) . . . . ?
O9 C52 Mo2 P2 134(18) . . . . ?
O10 C53 Mo2 C51 -21(7) . . . . ?
O10 C53 Mo2 C55 -33(9) . . . . ?
O10 C53 Mo2 C52 68(7) . . . . ?
O10 C53 Mo2 C54 -111(7) . . . . ?
O10 C53 Mo2 P2 156(7) . . . . ?
O11 C54 Mo2 C51 1(11) . . . . ?
O11 C54 Mo2 C55 -85(11) . . . . ?
O11 C54 Mo2 C52 -32(14) . . . . ?
O11 C54 Mo2 C53 90(11) . . . . ?
O11 C54 Mo2 P2 -173(100) . . . . ?
C4 C1 O1 P1 176.7(3) . . . . ?
C2 C1 O1 P1 50.5(3) . . . . ?
C10 C1 O1 P1 -62.9(3) . . . . ?
C15 C25 O7 P2 -7.1(4) . . . . ?
C26 C25 O7 P2 167.0(3) . . . . ?
C56 C57 O13 C59 179.0(6) . . . . ?
C60 C59 O13 C57 175.4(6) . . . . ?
C1 O1 P1 C3 -46.0(2) . . . . ?
C1 O1 P1 C11 49.2(3) . . . . ?
C1 O1 P1 Mo1 -179.99(18) . . . . ?
C2 C3 P1 O1 28.2(3) . . . . ?
C19 C3 P1 O1 -156.9(4) . . . . ?
C2 C3 P1 C11 -64.4(3) . . . . ?
C19 C3 P1 C11 110.4(4) . . . . ?
C2 C3 P1 Mo1 160.4(2) . . . . ?
C19 C3 P1 Mo1 -24.8(5) . . . . ?
C12 C11 P1 O1 -143.1(3) . . . . ?
C10 C11 P1 O1 -19.2(3) . . . . ?
C12 C11 P1 C3 -51.4(3) . . . . ?
C10 C11 P1 C3 72.5(3) . . . . ?
C12 C11 P1 Mo1 85.8(3) . . . . ?
C10 C11 P1 Mo1 -150.35(19) . . . . ?
C20 Mo1 P1 O1 -121(3) . . . . ?
C23 Mo1 P1 O1 -89.71(19) . . . . ?
C22 Mo1 P1 O1 -179.41(18) . . . . ?
C21 Mo1 P1 O1 89.68(19) . . . . ?
C24 Mo1 P1 O1 2.73(19) . . . . ?
C20 Mo1 P1 C3 120(3) . . . . ?
C23 Mo1 P1 C3 151.6(2) . . . . ?
C22 Mo1 P1 C3 61.9(2) . . . . ?
C21 Mo1 P1 C3 -29.0(2) . . . . ?
C24 Mo1 P1 C3 -116.0(2) . . . . ?
C20 Mo1 P1 C11 -4(3) . . . . ?
C23 Mo1 P1 C11 27.3(2) . . . . ?
C22 Mo1 P1 C11 -62.4(2) . . . . ?
C21 Mo1 P1 C11 -153.3(2) . . . . ?
C24 Mo1 P1 C11 119.8(2) . . . . ?
C25 O7 P2 C14 6.9(3) . . . . ?
C25 O7 P2 C32 -106.4(3) . . . . ?
C25 O7 P2 Mo2 119.7(2) . . . . ?
C13 C14 P2 O7 -131.1(3) . . . . ?
C15 C14 P2 O7 -5.0(3) . . . . ?
C13 C14 P2 C32 -26.1(4) . . . . ?
C15 C14 P2 C32 100.0(3) . . . . ?
C13 C14 P2 Mo2 115.4(3) . . . . ?
C15 C14 P2 Mo2 -118.5(2) . . . . ?
C39 C32 P2 O7 24.8(3) . . . . ?
C33 C32 P2 O7 147.7(2) . . . . ?
C45 C32 P2 O7 -94.9(3) . . . . ?
C39 C32 P2 C14 -73.9(3) . . . . ?
C33 C32 P2 C14 49.0(3) . . . . ?
C45 C32 P2 C14 166.4(3) . . . . ?
C39 C32 P2 Mo2 150.7(2) . . . . ?
C33 C32 P2 Mo2 -86.4(3) . . . . ?
C45 C32 P2 Mo2 31.0(3) . . . . ?
C51 Mo2 P2 O7 -74.2(16) . . . . ?
C55 Mo2 P2 O7 -48.26(18) . . . . ?
C52 Mo2 P2 O7 -138.37(17) . . . . ?
C53 Mo2 P2 O7 130.92(16) . . . . ?
C54 Mo2 P2 O7 40.34(17) . . . . ?
C51 Mo2 P2 C14 27.4(16) . . . . ?
C55 Mo2 P2 C14 53.3(2) . . . . ?
C52 Mo2 P2 C14 -36.78(19) . . . . ?
C53 Mo2 P2 C14 -127.49(19) . . . . ?
C54 Mo2 P2 C14 141.93(19) . . . . ?
C51 Mo2 P2 C32 163.5(16) . . . . ?
C55 Mo2 P2 C32 -170.6(2) . . . . ?
C52 Mo2 P2 C32 99.3(2) . . . . ?
C53 Mo2 P2 C32 8.60(19) . . . . ?
C54 Mo2 P2 C32 -82.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.893
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.104
####################################################################### 
# 
# 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_3425f
_database_code_depnum_ccdc_archive 'CCDC 1423354'
_audit_update_record             
;
2015-09-10 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_audit_creation_date             2014-05-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C37 H25 O6 P W'
_chemical_formula_sum            'C37 H25 O6 P W'
_chemical_formula_weight         780.39
_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'
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   9.4174(14)
_cell_length_b                   10.7473(14)
_cell_length_c                   17.631(2)
_cell_angle_alpha                98.301(4)
_cell_angle_beta                 94.830(4)
_cell_angle_gamma                112.865(4)
_cell_volume                     1607.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1853
_cell_measurement_temperature    123
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.45
_exptl_absorpt_coefficient_mu    3.688
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5374
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
Estimated minimum and maximum transmission:  0.5374  0.7460
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_av_unetI/netI     0.1408
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14721
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.73
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_reflns_number_gt                4003
_reflns_number_total             5711
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.268
_refine_diff_density_min         -1.704
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5711
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0498
_refine_ls_restrained_S_all      0.961
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0112P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0809
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
W W 0.67931(5) 0.33497(4) 0.11762(2) 0.01728(10) Uani 1 d . . . .
P P 0.9146(2) 0.4029(2) 0.21827(11) 0.0149(5) Uani 1 d . . . .
O1 O 0.9279(6) 0.5335(5) 0.2840(3) 0.0135(12) Uani 1 d . . . .
O2 O 0.3889(7) 0.2734(7) -0.0078(3) 0.0472(18) Uani 1 d . . . .
O3 O 0.4969(7) 0.0267(6) 0.1377(3) 0.0343(16) Uani 1 d . . . .
O4 O 0.8524(8) 0.2361(6) -0.0103(3) 0.0426(18) Uani 1 d . . . .
O5 O 0.8414(7) 0.6308(6) 0.0739(3) 0.0366(16) Uani 1 d . . . .
O6 O 0.5322(7) 0.4544(6) 0.2505(3) 0.0345(16) Uani 1 d . . . .
C1 C 1.0942(9) 0.5002(7) 0.1858(4) 0.0149(18) Uani 1 d . . . .
C2 C 1.1378(9) 0.6401(8) 0.2177(4) 0.0152(18) Uani 1 d . . . .
C3 C 1.0207(9) 0.6673(7) 0.2646(4) 0.0157(18) Uani 1 d . . . .
H3 H 0.9504 0.6924 0.2301 0.019 Uiso 1 calc . . R .
C4 C 1.1815(9) 0.4612(8) 0.1372(4) 0.0197(19) Uani 1 d . . . .
H4 H 1.1494 0.3669 0.1144 0.024 Uiso 1 calc . . R .
C5 C 1.3171(10) 0.5593(8) 0.1211(4) 0.0172(19) Uani 1 d . . . .
H5 H 1.3791 0.5321 0.0882 0.021 Uiso 1 calc . . R .
C6 C 1.3626(9) 0.6990(8) 0.1535(4) 0.022(2) Uani 1 d . . . .
H6 H 1.4572 0.7658 0.1438 0.027 Uiso 1 calc . . R .
C7 C 1.2700(9) 0.7397(7) 0.1997(4) 0.0176(18) Uani 1 d . . . .
H7 H 1.2968 0.8346 0.2186 0.021 Uiso 1 calc . . R .
C8 C 1.0833(9) 0.7749(7) 0.3373(4) 0.0174(18) Uani 1 d . . . .
C9 C 1.1650(9) 0.7599(7) 0.4017(4) 0.0187(19) Uani 1 d . . . .
H9 H 1.1832 0.6789 0.4014 0.022 Uiso 1 calc . . R .
C10 C 1.2197(10) 0.8637(8) 0.4663(4) 0.025(2) Uani 1 d . . . .
H10 H 1.2768 0.8535 0.5102 0.030 Uiso 1 calc . . R .
C11 C 1.1944(10) 0.9812(8) 0.4692(4) 0.026(2) Uani 1 d . . . .
H11 H 1.2326 1.0512 0.5145 0.031 Uiso 1 calc . . R .
C12 C 1.1140(11) 0.9961(9) 0.4062(5) 0.035(2) Uani 1 d . . . U
H12 H 1.0949 1.0769 0.4077 0.042 Uiso 1 calc . . R .
C13 C 1.0589(10) 0.8947(8) 0.3395(5) 0.027(2) Uani 1 d . . . .
H13 H 1.0046 0.9072 0.2953 0.032 Uiso 1 calc . . R .
C14 C 0.9562(8) 0.2850(7) 0.2804(4) 0.0145(17) Uani 1 d . . . .
C15 C 0.7992(9) 0.1970(7) 0.3039(4) 0.0167(18) Uani 1 d . . . .
C16 C 0.7012(9) 0.2573(8) 0.3288(4) 0.0178(19) Uani 1 d . . . .
H16 H 0.7315 0.3533 0.3318 0.021 Uiso 1 calc . . R .
C17 C 0.5592(9) 0.1789(8) 0.3496(4) 0.024(2) Uani 1 d . . . .
H17 H 0.4914 0.2207 0.3651 0.028 Uiso 1 calc . . R .
C18 C 0.5167(10) 0.0403(8) 0.3475(4) 0.024(2) Uani 1 d . . . .
H18 H 0.4200 -0.0132 0.3622 0.029 Uiso 1 calc . . R .
C19 C 0.6132(10) -0.0199(8) 0.3246(4) 0.024(2) Uani 1 d . . . .
H19 H 0.5837 -0.1154 0.3232 0.028 Uiso 1 calc . . R .
C20 C 0.7565(9) 0.0590(7) 0.3029(4) 0.0192(19) Uani 1 d . . . .
H20 H 0.8241 0.0168 0.2876 0.023 Uiso 1 calc . . R .
C21 C 1.0142(9) 0.1927(7) 0.2273(4) 0.0166(18) Uani 1 d . . . U
C22 C 0.9247(9) 0.1125(8) 0.1575(4) 0.0200(19) Uani 1 d . . . .
H22 H 0.8275 0.1165 0.1427 0.024 Uiso 1 calc . . R .
C23 C 0.9696(11) 0.0279(8) 0.1090(5) 0.031(2) Uani 1 d . . . .
H23 H 0.9036 -0.0263 0.0621 0.037 Uiso 1 calc . . R .
C24 C 1.1108(11) 0.0217(9) 0.1286(5) 0.034(2) Uani 1 d . . . .
H24 H 1.1445 -0.0347 0.0947 0.041 Uiso 1 calc . . R .
C25 C 1.2042(11) 0.0989(9) 0.1988(4) 0.032(2) Uani 1 d . . . .
H25 H 1.3010 0.0941 0.2135 0.039 Uiso 1 calc . . R .
C26 C 1.1549(9) 0.1825(8) 0.2466(4) 0.024(2) Uani 1 d . . . .
H26 H 1.2193 0.2348 0.2942 0.029 Uiso 1 calc . . R .
C27 C 1.0779(9) 0.3712(7) 0.3517(4) 0.0151(18) Uani 1 d . . . .
C28 C 1.0460(10) 0.3632(9) 0.4273(4) 0.026(2) Uani 1 d . . . .
H28 H 0.9435 0.3080 0.4349 0.031 Uiso 1 calc . . R .
C29 C 1.1610(11) 0.4341(9) 0.4916(4) 0.031(2) Uani 1 d . . . .
H29 H 1.1351 0.4272 0.5422 0.038 Uiso 1 calc . . R .
C30 C 1.3096(10) 0.5132(8) 0.4831(5) 0.029(2) Uani 1 d . . . .
H30 H 1.3878 0.5603 0.5272 0.035 Uiso 1 calc . . R .
C31 C 1.3448(10) 0.5236(8) 0.4085(5) 0.028(2) Uani 1 d . . . .
H31 H 1.4479 0.5788 0.4016 0.034 Uiso 1 calc . . R .
C32 C 1.2321(9) 0.4552(7) 0.3450(4) 0.0178(18) Uani 1 d . . . .
H32 H 1.2590 0.4647 0.2948 0.021 Uiso 1 calc . . R .
C33 C 0.4938(11) 0.2964(9) 0.0381(5) 0.031(2) Uani 1 d . . . .
C34 C 0.5685(10) 0.1399(9) 0.1336(4) 0.024(2) Uani 1 d . . . .
C35 C 0.7871(10) 0.2687(8) 0.0360(4) 0.021(2) Uani 1 d . . . U
C36 C 0.7838(10) 0.5259(9) 0.0914(4) 0.025(2) Uani 1 d . . . .
C37 C 0.5830(10) 0.4091(8) 0.2018(5) 0.022(2) Uani 1 d . . . .


_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
W P 2.510(2) . ?
W C33 2.012(9) . ?
W C34 2.021(9) . ?
W C35 2.030(9) . ?
W C36 2.043(9) . ?
W C37 2.027(9) . ?
P O1 1.642(5) . ?
P C1 1.801(7) . ?
P C14 1.916(7) . ?
O1 C3 1.471(7) . ?
O2 C33 1.144(10) . ?
O3 C34 1.155(9) . ?
O4 C35 1.156(9) . ?
O5 C36 1.146(8) . ?
O6 C37 1.154(9) . ?
C1 C2 1.408(9) . ?
C1 C4 1.367(9) . ?
C2 C3 1.523(9) . ?
C2 C7 1.388(10) . ?
C3 H3 1.0000 . ?
C3 C8 1.497(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.405(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(10) . ?
C8 C13 1.388(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.377(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.368(10) . ?
C11 H11 0.9500 . ?
C11 C12 1.355(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.389(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.544(10) . ?
C14 C21 1.548(10) . ?
C14 C27 1.533(10) . ?
C15 C16 1.384(10) . ?
C15 C20 1.374(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(10) . ?
C17 H17 0.9500 . ?
C17 C18 1.378(10) . ?
C18 H18 0.9500 . ?
C18 C19 1.360(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.406(10) . ?
C20 H20 0.9500 . ?
C21 C22 1.387(10) . ?
C21 C26 1.389(10) . ?
C22 H22 0.9500 . ?
C22 C23 1.368(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.375(11) . ?
C24 H24 0.9500 . ?
C24 C25 1.394(11) . ?
C25 H25 0.9500 . ?
C25 C26 1.380(10) . ?
C26 H26 0.9500 . ?
C27 C28 1.398(9) . ?
C27 C32 1.406(10) . ?
C28 H28 0.9500 . ?
C28 C29 1.394(11) . ?
C29 H29 0.9500 . ?
C29 C30 1.361(11) . ?
C30 H30 0.9500 . ?
C30 C31 1.393(10) . ?
C31 H31 0.9500 . ?
C31 C32 1.370(10) . ?
C32 H32 0.9500 . ?

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
C33 W P 175.5(3) . . ?
C33 W C34 87.0(3) . . ?
C33 W C35 91.4(3) . . ?
C33 W C36 89.1(3) . . ?
C33 W C37 91.0(3) . . ?
C34 W P 97.1(2) . . ?
C34 W C35 89.9(3) . . ?
C34 W C36 175.0(4) . . ?
C34 W C37 92.1(3) . . ?
C35 W P 90.6(2) . . ?
C35 W C36 87.2(3) . . ?
C36 W P 86.9(2) . . ?
C37 W P 86.9(2) . . ?
C37 W C35 176.9(4) . . ?
C37 W C36 91.0(3) . . ?
O1 P W 109.80(19) . . ?
O1 P C1 93.4(3) . . ?
O1 P C14 102.4(3) . . ?
C1 P W 112.9(2) . . ?
C1 P C14 107.3(3) . . ?
C14 P W 125.8(2) . . ?
C3 O1 P 112.7(4) . . ?
C2 C1 P 107.6(5) . . ?
C4 C1 P 131.8(6) . . ?
C4 C1 C2 120.6(7) . . ?
C1 C2 C3 114.0(6) . . ?
C7 C2 C1 120.0(7) . . ?
C7 C2 C3 125.8(7) . . ?
O1 C3 C2 104.4(5) . . ?
O1 C3 H3 108.3 . . ?
O1 C3 C8 109.5(5) . . ?
C2 C3 H3 108.3 . . ?
C8 C3 C2 117.7(6) . . ?
C8 C3 H3 108.3 . . ?
C1 C4 H4 120.0 . . ?
C1 C4 C5 119.9(7) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.9(7) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.3(7) . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C6 119.2(7) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C3 122.5(7) . . ?
C9 C8 C13 119.0(7) . . ?
C13 C8 C3 118.4(7) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.2(7) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 119.0 . . ?
C11 C10 C9 122.0(8) . . ?
C11 C10 H10 119.0 . . ?
C10 C11 H11 120.6 . . ?
C12 C11 C10 118.9(8) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 H12 119.6 . . ?
C11 C12 C13 120.9(7) . . ?
C13 C12 H12 119.6 . . ?
C8 C13 C12 120.0(8) . . ?
C8 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 P 106.4(5) . . ?
C15 C14 C21 110.4(6) . . ?
C21 C14 P 106.3(4) . . ?
C27 C14 P 110.1(5) . . ?
C27 C14 C15 111.4(6) . . ?
C27 C14 C21 111.9(6) . . ?
C16 C15 C14 120.2(7) . . ?
C20 C15 C14 120.8(7) . . ?
C20 C15 C16 118.9(7) . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.7(7) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 119.9(8) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.0(8) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.2(7) . . ?
C20 C19 H19 119.9 . . ?
C15 C20 C19 120.2(7) . . ?
C15 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C14 120.9(7) . . ?
C22 C21 C26 116.1(7) . . ?
C26 C21 C14 123.0(7) . . ?
C21 C22 H22 118.4 . . ?
C23 C22 C21 123.2(8) . . ?
C23 C22 H22 118.4 . . ?
C22 C23 H23 120.2 . . ?
C22 C23 C24 119.6(8) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 120.3 . . ?
C23 C24 C25 119.4(8) . . ?
C25 C24 H24 120.3 . . ?
C24 C25 H25 120.2 . . ?
C26 C25 C24 119.5(8) . . ?
C26 C25 H25 120.2 . . ?
C21 C26 H26 118.9 . . ?
C25 C26 C21 122.2(8) . . ?
C25 C26 H26 118.9 . . ?
C28 C27 C14 122.1(7) . . ?
C28 C27 C32 115.9(7) . . ?
C32 C27 C14 121.9(6) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 C27 121.6(8) . . ?
C29 C28 H28 119.2 . . ?
C28 C29 H29 119.5 . . ?
C30 C29 C28 121.1(8) . . ?
C30 C29 H29 119.5 . . ?
C29 C30 H30 120.7 . . ?
C29 C30 C31 118.6(8) . . ?
C31 C30 H30 120.7 . . ?
C30 C31 H31 119.7 . . ?
C32 C31 C30 120.6(8) . . ?
C32 C31 H31 119.7 . . ?
C27 C32 H32 118.9 . . ?
C31 C32 C27 122.2(7) . . ?
C31 C32 H32 118.9 . . ?
O2 C33 W 179.0(8) . . ?
O3 C34 W 174.7(8) . . ?
O4 C35 W 177.4(7) . . ?
O5 C36 W 177.6(7) . . ?
O6 C37 W 178.1(8) . . ?

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
W P O1 C3 -90.2(4) . . . . ?
W P C1 C2 100.6(5) . . . . ?
W P C1 C4 -77.0(7) . . . . ?
W P C14 C15 -40.4(6) . . . . ?
W P C14 C21 77.3(5) . . . . ?
W P C14 C27 -161.3(4) . . . . ?
P W C33 O2 131(51) . . . . ?
P W C34 O3 -172(8) . . . . ?
P W C35 O4 -67(15) . . . . ?
P W C36 O5 131(17) . . . . ?
P W C37 O6 42(20) . . . . ?
P O1 C3 C2 -29.7(6) . . . . ?
P O1 C3 C8 -156.6(5) . . . . ?
P C1 C2 C3 -3.1(7) . . . . ?
P C1 C2 C7 -177.5(6) . . . . ?
P C1 C4 C5 179.4(6) . . . . ?
P C14 C15 C16 -43.9(8) . . . . ?
P C14 C15 C20 138.3(6) . . . . ?
P C14 C21 C22 -56.1(8) . . . . ?
P C14 C21 C26 125.3(6) . . . . ?
P C14 C27 C28 120.1(6) . . . . ?
P C14 C27 C32 -65.0(8) . . . . ?
O1 P C1 C2 -12.6(5) . . . . ?
O1 P C1 C4 169.9(7) . . . . ?
O1 P C14 C15 85.5(5) . . . . ?
O1 P C14 C21 -156.9(5) . . . . ?
O1 P C14 C27 -35.4(5) . . . . ?
O1 C3 C8 C9 52.1(9) . . . . ?
O1 C3 C8 C13 -128.3(7) . . . . ?
C1 P O1 C3 25.6(5) . . . . ?
C1 P C14 C15 -177.0(5) . . . . ?
C1 P C14 C21 -59.3(6) . . . . ?
C1 P C14 C27 62.1(6) . . . . ?
C1 C2 C3 O1 19.7(8) . . . . ?
C1 C2 C3 C8 141.3(6) . . . . ?
C1 C2 C7 C6 -3.6(11) . . . . ?
C1 C4 C5 C6 -1.4(11) . . . . ?
C2 C1 C4 C5 2.2(11) . . . . ?
C2 C3 C8 C9 -66.9(9) . . . . ?
C2 C3 C8 C13 112.7(8) . . . . ?
C3 C2 C7 C6 -177.3(6) . . . . ?
C3 C8 C9 C10 179.7(7) . . . . ?
C3 C8 C13 C12 179.3(7) . . . . ?
C4 C1 C2 C3 174.8(6) . . . . ?
C4 C1 C2 C7 0.3(11) . . . . ?
C4 C5 C6 C7 -2.0(11) . . . . ?
C5 C6 C7 C2 4.4(11) . . . . ?
C7 C2 C3 O1 -166.2(7) . . . . ?
C7 C2 C3 C8 -44.6(10) . . . . ?
C8 C9 C10 C11 0.7(12) . . . . ?
C9 C8 C13 C12 -1.1(12) . . . . ?
C9 C10 C11 C12 -0.5(12) . . . . ?
C10 C11 C12 C13 -0.5(13) . . . . ?
C11 C12 C13 C8 1.3(13) . . . . ?
C13 C8 C9 C10 0.1(11) . . . . ?
C14 P O1 C3 134.1(5) . . . . ?
C14 P C1 C2 -116.7(5) . . . . ?
C14 P C1 C4 65.8(8) . . . . ?
C14 C15 C16 C17 179.5(7) . . . . ?
C14 C15 C20 C19 179.9(7) . . . . ?
C14 C21 C22 C23 -179.1(6) . . . . ?
C14 C21 C26 C25 179.6(7) . . . . ?
C14 C27 C28 C29 175.1(7) . . . . ?
C14 C27 C32 C31 -174.5(7) . . . . ?
C15 C14 C21 C22 59.0(8) . . . . ?
C15 C14 C21 C26 -119.7(8) . . . . ?
C15 C14 C27 C28 2.2(10) . . . . ?
C15 C14 C27 C32 177.2(6) . . . . ?
C15 C16 C17 C18 1.9(11) . . . . ?
C16 C15 C20 C19 2.1(11) . . . . ?
C16 C17 C18 C19 -0.6(12) . . . . ?
C17 C18 C19 C20 0.0(12) . . . . ?
C18 C19 C20 C15 -0.8(12) . . . . ?
C20 C15 C16 C17 -2.6(11) . . . . ?
C21 C14 C15 C16 -158.9(6) . . . . ?
C21 C14 C15 C20 23.3(10) . . . . ?
C21 C14 C27 C28 -121.9(7) . . . . ?
C21 C14 C27 C32 53.1(8) . . . . ?
C21 C22 C23 C24 -0.9(12) . . . . ?
C22 C21 C26 C25 0.8(11) . . . . ?
C22 C23 C24 C25 1.8(13) . . . . ?
C23 C24 C25 C26 -1.4(13) . . . . ?
C24 C25 C26 C21 0.0(12) . . . . ?
C26 C21 C22 C23 -0.4(11) . . . . ?
C27 C14 C15 C16 76.1(8) . . . . ?
C27 C14 C15 C20 -101.7(8) . . . . ?
C27 C14 C21 C22 -176.3(6) . . . . ?
C27 C14 C21 C26 5.0(9) . . . . ?
C27 C28 C29 C30 -0.7(13) . . . . ?
C28 C27 C32 C31 0.7(11) . . . . ?
C28 C29 C30 C31 0.9(12) . . . . ?
C29 C30 C31 C32 -0.3(12) . . . . ?
C30 C31 C32 C27 -0.5(12) . . . . ?
C32 C27 C28 C29 -0.2(11) . . . . ?
C33 W P O1 34(3) . . . . ?
C33 W P C1 -69(3) . . . . ?
C33 W P C14 157(3) . . . . ?
C33 W C34 O3 10(8) . . . . ?
C33 W C35 O4 109(15) . . . . ?
C33 W C36 O5 -51(17) . . . . ?
C33 W C37 O6 -134(20) . . . . ?
C34 W P O1 -119.9(3) . . . . ?
C34 W P C1 137.4(3) . . . . ?
C34 W P C14 2.8(4) . . . . ?
C34 W C33 O2 -74(52) . . . . ?
C34 W C35 O4 -164(15) . . . . ?
C34 W C36 O5 -14(20) . . . . ?
C34 W C37 O6 139(20) . . . . ?
C35 W P O1 150.2(3) . . . . ?
C35 W P C1 47.4(3) . . . . ?
C35 W P C14 -87.2(3) . . . . ?
C35 W C33 O2 15(52) . . . . ?
C35 W C34 O3 -82(8) . . . . ?
C35 W C36 O5 40(17) . . . . ?
C35 W C37 O6 8(25) . . . . ?
C36 W P O1 63.0(3) . . . . ?
C36 W P C1 -39.7(3) . . . . ?
C36 W P C14 -174.3(4) . . . . ?
C36 W C33 O2 103(52) . . . . ?
C36 W C34 O3 -28(11) . . . . ?
C36 W C35 O4 20(15) . . . . ?
C36 W C37 O6 -45(20) . . . . ?
C37 W P O1 -28.1(3) . . . . ?
C37 W P C1 -130.9(3) . . . . ?
C37 W P C14 94.6(3) . . . . ?
C37 W C33 O2 -166(52) . . . . ?
C37 W C34 O3 101(8) . . . . ?
C37 W C35 O4 -34(19) . . . . ?
C37 W C36 O5 -142(17) . . . . ?

