# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2005


data_global
_journal_name_full               'New J.Chem.(Nouv.J.Chim.)'

_journal_coden_Cambridge         0440
_publ_contact_author_name        'Konstantin Rufanov'

_publ_contact_author_address     
;
Leibniz-Institut fur Organische Katalyse an der Universitat Rostock
Albert-Einstein-Strasse 29A
Rostock
18059
GERMANY
;

_publ_contact_author_email       Konstantin.Rufanov@ifok-rostock.de
loop_
_publ_author_name
'K.A. Rufanov'
'B.H. Muller'
'A. Spannenberg'
'U. Rosenthal'

_publ_section_title              
;
Synthesis and Molecular Structures of the First
Phosphoranylidene Complexes of the Rare-Earth (Y, Lu) Metals
;

data_ruf2a
_database_code_depnum_ccdc_archive 'CCDC 245412'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'Lutetium betain-complex'
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H56 Lu2 O4 P2, 4(C6 H6)'
_chemical_formula_sum            'C84 H80 Lu2 O4 P2'
_chemical_formula_weight         1565.36

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'
Lu Lu -0.4720 5.8584 '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'

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                   14.192(5)
_cell_length_b                   12.461(4)
_cell_length_c                   20.490(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.51(3)
_cell_angle_gamma                90.00
_cell_volume                     3491.6(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    5000
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      23.0

_exptl_crystal_description       block
_exptl_crystal_colour            light-yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1576
_exptl_absorpt_coefficient_mu    2.908
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_process_details   
;
The correction was carried out by ABSCOR (Stoe, 1997), a modification of
DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166.
In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones.
;

_exptl_special_details           
;
During data collection the crystal was in cold N~2~ gas of the Cryostream
Cooler (Oxford Cryosystems) mounted on a \f-axis diffractometer
supplied with an area detector.
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-oscill.,\f-incr.=1.4\%,157 exposures'
_diffrn_detector_area_resol_mean 6.667
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            17113
_diffrn_reflns_av_R_equivalents  0.2200
_diffrn_reflns_av_sigmaI/netI    0.1849
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         23.26
_reflns_number_total             4979
_reflns_number_gt                2802
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (Stoe & Cie, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'

_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^ > 2sigma(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^)+(0.1598P)^2^] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.0019(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4979
_refine_ls_number_parameters     393
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0843
_refine_ls_wR_factor_ref         0.2278
_refine_ls_wR_factor_gt          0.1929
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_restrained_S_all      0.928
_refine_ls_shift/su_max          0.005
_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 0.0288(12) 0.0835(11) 1.0668(8) 0.049(3) Uani 1 1 d . . .
C2 C 0.1035(16) 0.0496(13) 1.1299(10) 0.062(5) Uani 1 1 d . . .
C3 C 0.1940(17) 0.0160(13) 1.1256(10) 0.065(5) Uani 1 1 d . . .
C4 C 0.2661(16) -0.0230(16) 1.1811(11) 0.070(5) Uani 1 1 d . . .
H4 H 0.3281 -0.0428 1.1755 0.084 Uiso 1 1 calc R . .
C5 C 0.2484(16) -0.0333(16) 1.2444(11) 0.072(5) Uani 1 1 d . . .
H5 H 0.2960 -0.0632 1.2817 0.086 Uiso 1 1 calc R . .
C6 C 0.1537(18) 0.0036(17) 1.2512(12) 0.078(6) Uani 1 1 d . . .
H6 H 0.1387 0.0021 1.2936 0.094 Uiso 1 1 calc R . .
C7 C 0.0878(16) 0.0400(16) 1.1946(9) 0.064(5) Uani 1 1 d . . .
H7 H 0.0255 0.0609 1.1991 0.077 Uiso 1 1 calc R . .
C8 C 0.3039(18) -0.005(2) 1.0538(13) 0.081(6) Uani 1 1 d . . .
H8A H 0.3053 0.0049 1.0066 0.122 Uiso 1 1 calc R . .
H8B H 0.3150 -0.0808 1.0662 0.122 Uiso 1 1 calc R . .
H8C H 0.3554 0.0387 1.0834 0.122 Uiso 1 1 calc R . .
C9 C 0.236(2) 0.2755(19) 1.0215(15) 0.097(8) Uani 1 1 d . . .
H9A H 0.3002 0.2396 1.0357 0.116 Uiso 1 1 calc R . .
H9B H 0.2031 0.2662 1.0582 0.116 Uiso 1 1 calc R . .
C10 C 0.250(3) 0.389(2) 1.0115(19) 0.133(13) Uani 1 1 d . . .
H10A H 0.3191 0.4098 1.0303 0.160 Uiso 1 1 calc R . .
H10B H 0.2083 0.4333 1.0328 0.160 Uiso 1 1 calc R . .
C11 C 0.220(3) 0.399(2) 0.9372(19) 0.127(12) Uani 1 1 d . . .
H11A H 0.2777 0.4105 0.9199 0.153 Uiso 1 1 calc R . .
H11B H 0.1756 0.4617 0.9239 0.153 Uiso 1 1 calc R . .
C12 C 0.167(2) 0.2974(17) 0.9073(12) 0.083(7) Uani 1 1 d . . .
H12A H 0.0968 0.3116 0.8863 0.100 Uiso 1 1 calc R . .
H12B H 0.1963 0.2670 0.8726 0.100 Uiso 1 1 calc R . .
C13 C 0.1620(14) -0.0229(11) 0.8952(9) 0.053(4) Uani 1 1 d . . .
C14 C 0.1492(16) -0.1365(13) 0.8927(10) 0.061(5) Uani 1 1 d . . .
C15 C 0.2019(16) -0.2059(17) 0.8604(10) 0.070(5) Uani 1 1 d . . .
H15 H 0.1856 -0.2800 0.8560 0.084 Uiso 1 1 calc R . .
C16 C 0.2768(16) -0.1674(19) 0.8353(11) 0.074(5) Uani 1 1 d . . .
H16 H 0.3129 -0.2133 0.8139 0.089 Uiso 1 1 calc R . .
C17 C 0.2963(17) -0.0591(17) 0.8430(12) 0.077(6) Uani 1 1 d . . .
H17 H 0.3497 -0.0319 0.8282 0.092 Uiso 1 1 calc R . .
C18 C 0.2455(15) 0.0099(17) 0.8698(11) 0.071(5) Uani 1 1 d . . .
H18 H 0.2638 0.0834 0.8726 0.085 Uiso 1 1 calc R . .
C19 C 0.1086(14) -0.2216(13) 1.0122(11) 0.063(5) Uani 1 1 d . . .
C20 C 0.2014(17) -0.2785(14) 1.0297(12) 0.075(6) Uani 1 1 d . . .
H20 H 0.2313 -0.2932 0.9943 0.090 Uiso 1 1 calc R . .
C21 C 0.2489(14) -0.3126(15) 1.0937(11) 0.068(5) Uani 1 1 d . . .
H21 H 0.3098 -0.3492 1.1028 0.081 Uiso 1 1 calc R . .
C22 C 0.2023(15) -0.2905(13) 1.1460(11) 0.067(5) Uani 1 1 d . . .
H22 H 0.2315 -0.3146 1.1908 0.081 Uiso 1 1 calc R . .
C23 C 0.111(2) -0.2315(15) 1.1314(11) 0.080(6) Uani 1 1 d . . .
H23 H 0.0831 -0.2147 1.1677 0.096 Uiso 1 1 calc R . .
C24 C 0.0624(14) -0.1992(12) 1.0674(9) 0.053(4) Uani 1 1 d . . .
C25 C 0.0020(15) -0.3005(14) 0.8826(12) 0.067(5) Uani 1 1 d . . .
C26 C -0.0187(18) -0.3045(16) 0.8125(11) 0.075(6) Uani 1 1 d . . .
H26 H -0.0044 -0.2441 0.7885 0.090 Uiso 1 1 calc R . .
C27 C -0.0598(16) -0.3952(15) 0.7771(11) 0.069(5) Uani 1 1 d . . .
H27 H -0.0752 -0.3960 0.7290 0.083 Uiso 1 1 calc R . .
C28 C -0.0781(17) -0.4832(17) 0.8110(13) 0.082(7) Uani 1 1 d . . .
H28 H -0.1074 -0.5452 0.7869 0.098 Uiso 1 1 calc R . .
C29 C -0.0534(16) -0.4815(13) 0.8816(11) 0.067(5) Uani 1 1 d . . .
H29 H -0.0638 -0.5441 0.9052 0.080 Uiso 1 1 calc R . .
C30 C -0.0146(18) -0.3917(14) 0.9180(12) 0.074(6) Uani 1 1 d . . .
H30 H 0.0007 -0.3915 0.9661 0.089 Uiso 1 1 calc R . .
C31 C 0.454(2) -0.316(3) 0.9860(15) 0.17(2) Uani 1 1 d G . .
H31 H 0.4207 -0.3504 0.9449 0.203 Uiso 1 1 calc R . .
C32 C 0.482(2) -0.3742(19) 1.0458(19) 0.160(17) Uani 1 1 d G . .
H32 H 0.4684 -0.4489 1.0456 0.192 Uiso 1 1 calc R . .
C33 C 0.530(2) -0.323(2) 1.1059(14) 0.138(13) Uani 1 1 d G . .
H33 H 0.5495 -0.3634 1.1467 0.166 Uiso 1 1 calc R . .
C34 C 0.550(2) -0.214(2) 1.1061(12) 0.149(16) Uani 1 1 d G . .
H34 H 0.5828 -0.1795 1.1472 0.179 Uiso 1 1 calc R . .
C35 C 0.521(2) -0.1557(18) 1.0463(16) 0.132(12) Uani 1 1 d G . .
H35 H 0.5350 -0.0810 1.0465 0.158 Uiso 1 1 calc R . .
C36 C 0.473(2) -0.206(3) 0.9862(12) 0.18(2) Uani 1 1 d G . .
H36 H 0.4539 -0.1664 0.9453 0.213 Uiso 1 1 calc R . .
C37 C 0.428(4) 0.2186(17) 1.2143(15) 0.17(2) Uani 1 1 d G . .
H37 H 0.4424 0.1443 1.2208 0.209 Uiso 1 1 calc R . .
C38 C 0.502(2) 0.291(3) 1.2141(16) 0.18(2) Uani 1 1 d G . .
H38 H 0.5673 0.2667 1.2205 0.213 Uiso 1 1 calc R . .
C39 C 0.4809(16) 0.400(3) 1.2046(14) 0.17(2) Uani 1 1 d G . .
H39 H 0.5316 0.4497 1.2045 0.210 Uiso 1 1 calc R . .
C40 C 0.385(2) 0.4360(17) 1.1952(12) 0.142(17) Uani 1 1 d G . .
H40 H 0.3710 0.5103 1.1887 0.170 Uiso 1 1 calc R . .
C41 C 0.3113(13) 0.363(3) 1.1954(12) 0.138(16) Uani 1 1 d G . .
H41 H 0.2461 0.3879 1.1890 0.165 Uiso 1 1 calc R . .
C42 C 0.332(3) 0.255(3) 1.2049(14) 0.20(3) Uani 1 1 d G . .
H42 H 0.2818 0.2049 1.2050 0.239 Uiso 1 1 calc R . .
O1 O 0.2106(10) 0.0276(10) 1.0613(7) 0.067(3) Uani 1 1 d . . .
O2 O 0.1793(12) 0.2271(9) 0.9625(8) 0.081(4) Uani 1 1 d . . .
P P 0.0534(4) -0.1794(3) 0.9295(3) 0.0587(11) Uani 1 1 d . . .
Lu Lu 0.07525(6) 0.07968(5) 0.96466(4) 0.0556(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.076(10) 0.025(6) 0.042(8) -0.008(6) 0.008(7) -0.017(7)
C2 0.084(13) 0.042(8) 0.063(12) -0.009(7) 0.023(10) -0.003(8)
C3 0.096(15) 0.041(8) 0.055(11) -0.005(7) 0.017(11) -0.010(9)
C4 0.069(12) 0.064(11) 0.066(13) -0.003(9) 0.000(10) -0.010(9)
C5 0.079(13) 0.069(11) 0.060(12) 0.026(9) 0.006(10) 0.025(10)
C6 0.094(16) 0.067(11) 0.074(15) -0.004(10) 0.023(13) -0.005(11)
C7 0.071(12) 0.071(11) 0.042(10) 0.003(8) 0.003(9) 0.005(9)
C8 0.083(15) 0.085(14) 0.077(15) 0.008(11) 0.024(12) 0.003(12)
C9 0.100(18) 0.070(13) 0.100(19) -0.003(12) -0.009(15) -0.032(12)
C10 0.20(4) 0.074(15) 0.12(3) -0.017(16) 0.03(3) -0.06(2)
C11 0.17(3) 0.086(18) 0.11(3) 0.016(17) 0.01(2) -0.015(19)
C12 0.109(18) 0.062(11) 0.083(16) 0.014(10) 0.033(14) -0.020(11)
C13 0.072(11) 0.031(7) 0.059(11) -0.010(6) 0.021(9) 0.015(7)
C14 0.083(13) 0.046(9) 0.061(11) 0.007(7) 0.032(10) 0.002(8)
C15 0.080(14) 0.068(11) 0.060(12) -0.007(9) 0.015(10) 0.002(10)
C16 0.070(13) 0.086(14) 0.067(13) -0.014(10) 0.022(11) 0.005(10)
C17 0.080(14) 0.078(13) 0.078(14) -0.001(10) 0.032(12) -0.011(10)
C18 0.072(13) 0.065(11) 0.078(14) -0.001(10) 0.023(11) -0.022(9)
C19 0.064(11) 0.050(9) 0.087(14) -0.008(9) 0.039(10) -0.004(8)
C20 0.088(14) 0.042(8) 0.093(16) 0.013(9) 0.018(12) 0.027(9)
C21 0.056(11) 0.061(10) 0.073(13) 0.019(9) -0.005(10) -0.004(8)
C22 0.074(13) 0.042(8) 0.077(14) 0.008(8) 0.006(11) 0.005(8)
C23 0.14(2) 0.044(9) 0.062(13) -0.006(8) 0.026(13) -0.004(11)
C24 0.072(11) 0.043(7) 0.044(10) 0.000(7) 0.014(8) -0.002(7)
C25 0.073(12) 0.047(8) 0.088(15) -0.012(9) 0.033(11) 0.002(8)
C26 0.104(17) 0.060(10) 0.065(13) -0.012(9) 0.031(12) -0.010(10)
C27 0.084(13) 0.059(10) 0.068(13) -0.019(9) 0.024(11) -0.009(9)
C28 0.077(14) 0.067(12) 0.093(18) -0.034(12) 0.008(12) -0.013(10)
C29 0.084(13) 0.036(8) 0.076(14) -0.002(8) 0.016(11) 0.010(8)
C30 0.101(16) 0.044(9) 0.077(14) -0.006(8) 0.023(12) -0.014(9)
C31 0.10(3) 0.20(5) 0.18(5) -0.10(4) 0.00(3) 0.00(3)
C32 0.13(3) 0.18(4) 0.17(4) -0.02(4) 0.05(3) -0.05(3)
C33 0.16(4) 0.16(3) 0.10(3) 0.02(2) 0.04(2) 0.00(3)
C34 0.18(4) 0.12(3) 0.13(3) 0.02(2) 0.03(3) -0.07(3)
C35 0.11(3) 0.14(3) 0.14(3) 0.01(3) 0.02(2) 0.01(2)
C36 0.16(4) 0.17(4) 0.18(5) 0.05(4) 0.00(4) 0.00(3)
C37 0.26(7) 0.09(2) 0.17(5) -0.04(2) 0.05(5) 0.01(3)
C38 0.18(5) 0.21(5) 0.18(4) 0.05(4) 0.10(4) 0.08(4)
C39 0.064(17) 0.30(7) 0.15(3) 0.11(4) 0.009(18) -0.02(3)
C40 0.22(5) 0.079(17) 0.09(2) -0.010(15) -0.02(3) 0.04(2)
C41 0.068(16) 0.25(5) 0.09(2) -0.02(3) 0.015(15) -0.01(2)
C42 0.36(10) 0.13(3) 0.11(3) -0.03(3) 0.06(4) -0.11(5)
O1 0.073(8) 0.059(7) 0.071(9) 0.003(6) 0.021(7) -0.002(6)
O2 0.108(11) 0.040(6) 0.098(11) -0.001(6) 0.034(9) -0.026(7)
P 0.077(3) 0.041(2) 0.057(3) -0.0068(18) 0.017(2) -0.002(2)
Lu 0.0742(5) 0.0384(4) 0.0551(5) -0.0010(4) 0.0190(3) -0.0020(4)

_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 1.50(3) . ?
C1 P 1.686(17) 3_557 ?
C1 Lu 2.358(15) . ?
C1 Lu 2.494(13) 3_557 ?
C2 C3 1.38(3) . ?
C2 C7 1.41(3) . ?
C3 C4 1.40(3) . ?
C3 O1 1.41(2) . ?
C4 C5 1.39(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.46(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.36(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 O1 1.43(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 O2 1.40(3) . ?
C9 C10 1.45(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.47(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.52(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O2 1.40(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.43(2) . ?
C13 C18 1.47(3) . ?
C13 Lu 2.472(14) . ?
C14 C15 1.42(3) . ?
C14 P 1.804(18) . ?
C15 C16 1.38(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.38(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.33(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.45(3) . ?
C19 C24 1.48(2) . ?
C19 P 1.75(2) . ?
C20 C21 1.37(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.43(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.46(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.37(3) . ?
C23 H23 0.9500 . ?
C24 Lu 2.404(18) 3_557 ?
C25 C26 1.39(3) . ?
C25 C30 1.40(3) . ?
C25 P 1.833(19) . ?
C26 C27 1.39(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.36(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.39(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.38(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C31 H31 0.9500 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33 0.9500 . ?
C34 C35 1.3900 . ?
C34 H34 0.9500 . ?
C35 C36 1.3900 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.3900 . ?
C37 C42 1.3900 . ?
C37 H37 0.9500 . ?
C38 C39 1.3900 . ?
C38 H38 0.9500 . ?
C39 C40 1.3900 . ?
C39 H39 0.9500 . ?
C40 C41 1.3900 . ?
C40 H40 0.9500 . ?
C41 C42 1.3900 . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
O1 Lu 2.449(15) . ?
O2 Lu 2.364(12) . ?
P C1 1.686(17) 3_557 ?
P Lu 3.305(4) . ?
Lu C24 2.404(18) 3_557 ?
Lu C1 2.494(13) 3_557 ?
Lu Lu 3.5011(16) 3_557 ?

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 P 120.0(11) . 3_557 ?
C2 C1 Lu 117.3(12) . . ?
P C1 Lu 114.5(8) 3_557 . ?
C2 C1 Lu 103.1(9) . 3_557 ?
P C1 Lu 102.8(7) 3_557 3_557 ?
Lu C1 Lu 92.3(5) . 3_557 ?
C3 C2 C7 114.8(19) . . ?
C3 C2 C1 119.2(17) . . ?
C7 C2 C1 125.7(18) . . ?
C2 C3 C4 123.1(19) . . ?
C2 C3 O1 114.9(18) . . ?
C4 C3 O1 122(2) . . ?
C5 C4 C3 121(2) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 117.3(19) . . ?
C4 C5 H5 121.4 . . ?
C6 C5 H5 121.4 . . ?
C7 C6 C5 118(2) . . ?
C7 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
C6 C7 C2 126(2) . . ?
C6 C7 H7 117.0 . . ?
C2 C7 H7 117.0 . . ?
O1 C8 H8A 109.5 . . ?
O1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C9 C10 112(2) . . ?
O2 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
O2 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C9 C10 C11 103(2) . . ?
C9 C10 H10A 111.2 . . ?
C11 C10 H10A 111.2 . . ?
C9 C10 H10B 111.2 . . ?
C11 C10 H10B 111.2 . . ?
H10A C10 H10B 109.2 . . ?
C10 C11 C12 109(2) . . ?
C10 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
C10 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
O2 C12 C11 105(2) . . ?
O2 C12 H12A 110.8 . . ?
C11 C12 H12A 110.8 . . ?
O2 C12 H12B 110.8 . . ?
C11 C12 H12B 110.8 . . ?
H12A C12 H12B 108.9 . . ?
C14 C13 C18 111.6(15) . . ?
C14 C13 Lu 117.1(13) . . ?
C18 C13 Lu 129.2(12) . . ?
C15 C14 C13 123.0(17) . . ?
C15 C14 P 124.4(14) . . ?
C13 C14 P 112.5(13) . . ?
C16 C15 C14 121.0(19) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C17 C16 C15 116.6(19) . . ?
C17 C16 H16 121.7 . . ?
C15 C16 H16 121.7 . . ?
C18 C17 C16 124(2) . . ?
C18 C17 H17 117.8 . . ?
C16 C17 H17 117.8 . . ?
C17 C18 C13 122.9(17) . . ?
C17 C18 H18 118.6 . . ?
C13 C18 H18 118.6 . . ?
C20 C19 C24 117(2) . . ?
C20 C19 P 121.9(15) . . ?
C24 C19 P 120.6(14) . . ?
C21 C20 C19 125(2) . . ?
C21 C20 H20 117.7 . . ?
C19 C20 H20 117.7 . . ?
C20 C21 C22 116.7(19) . . ?
C20 C21 H21 121.6 . . ?
C22 C21 H21 121.6 . . ?
C21 C22 C23 120.8(19) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C24 C23 C22 122(2) . . ?
C24 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C23 C24 C19 118.0(19) . . ?
C23 C24 Lu 127.2(14) . 3_557 ?
C19 C24 Lu 113.7(12) . 3_557 ?
C26 C25 C30 119.3(18) . . ?
C26 C25 P 121.1(15) . . ?
C30 C25 P 119.6(17) . . ?
C27 C26 C25 121(2) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C28 C27 C26 120(2) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 119.2(18) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 121.9(19) . . ?
C30 C29 H29 119.0 . . ?
C28 C29 H29 119.0 . . ?
C29 C30 C25 118(2) . . ?
C29 C30 H30 120.8 . . ?
C25 C30 H30 120.8 . . ?
C32 C31 C36 120.0 . . ?
C32 C31 H31 120.0 . . ?
C36 C31 H31 120.0 . . ?
C33 C32 C31 120.0 . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C31 120.0 . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?
C38 C37 C42 120.0 . . ?
C38 C37 H37 120.0 . . ?
C42 C37 H37 120.0 . . ?
C39 C38 C37 120.0 . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C39 C40 120.0 . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C39 C40 C41 120.0 . . ?
C39 C40 H40 120.0 . . ?
C41 C40 H40 120.0 . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C37 120.0 . . ?
C41 C42 H42 120.0 . . ?
C37 C42 H42 120.0 . . ?
C3 O1 C8 117.5(16) . . ?
C3 O1 Lu 119.5(12) . . ?
C8 O1 Lu 122.4(12) . . ?
C9 O2 C12 110.3(16) . . ?
C9 O2 Lu 122.4(14) . . ?
C12 O2 Lu 123.8(14) . . ?
C1 P C19 107.8(8) 3_557 . ?
C1 P C14 114.6(8) 3_557 . ?
C19 P C14 107.6(9) . . ?
C1 P C25 115.1(8) 3_557 . ?
C19 P C25 105.9(9) . . ?
C14 P C25 105.3(9) . . ?
C1 P Lu 47.4(5) 3_557 . ?
C19 P Lu 95.2(6) . . ?
C14 P Lu 76.3(6) . . ?
C25 P Lu 156.9(7) . . ?
C1 Lu O2 109.0(5) . . ?
C1 Lu C24 80.2(6) . 3_557 ?
O2 Lu C24 88.8(6) . 3_557 ?
C1 Lu O1 68.4(5) . . ?
O2 Lu O1 82.1(5) . . ?
C24 Lu O1 142.1(5) 3_557 . ?
C1 Lu C13 145.3(6) . . ?
O2 Lu C13 88.9(6) . . ?
C24 Lu C13 131.0(6) 3_557 . ?
O1 Lu C13 85.7(5) . . ?
C1 Lu C1 87.7(5) . 3_557 ?
O2 Lu C1 163.3(5) . 3_557 ?
C24 Lu C1 93.0(6) 3_557 3_557 ?
O1 Lu C1 106.0(5) . 3_557 ?
C13 Lu C1 77.4(6) . 3_557 ?
C1 Lu P 100.4(3) . . ?
O2 Lu P 141.0(4) . . ?
C24 Lu P 121.6(4) 3_557 . ?
O1 Lu P 85.7(3) . . ?
C13 Lu P 53.2(4) . . ?
C1 Lu P 29.8(4) 3_557 . ?
C1 Lu Lu 45.4(3) . 3_557 ?
O2 Lu Lu 154.4(4) . 3_557 ?
C24 Lu Lu 85.6(4) 3_557 3_557 ?
O1 Lu Lu 87.1(3) . 3_557 ?
C13 Lu Lu 113.4(4) . 3_557 ?
C1 Lu Lu 42.3(3) 3_557 3_557 ?
P Lu Lu 60.26(9) . 3_557 ?

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
P C1 C2 C3 -148.3(13) 3_557 . . . ?
Lu C1 C2 C3 -1.4(19) . . . . ?
Lu C1 C2 C3 98.3(15) 3_557 . . . ?
P C1 C2 C7 37(2) 3_557 . . . ?
Lu C1 C2 C7 -175.8(14) . . . . ?
Lu C1 C2 C7 -76.1(18) 3_557 . . . ?
C7 C2 C3 C4 -1(3) . . . . ?
C1 C2 C3 C4 -176.1(16) . . . . ?
C7 C2 C3 O1 -178.7(15) . . . . ?
C1 C2 C3 O1 6(2) . . . . ?
C2 C3 C4 C5 2(3) . . . . ?
O1 C3 C4 C5 179.6(18) . . . . ?
C3 C4 C5 C6 -3(3) . . . . ?
C4 C5 C6 C7 3(3) . . . . ?
C5 C6 C7 C2 -3(3) . . . . ?
C3 C2 C7 C6 1(3) . . . . ?
C1 C2 C7 C6 176.1(18) . . . . ?
O2 C9 C10 C11 -14(4) . . . . ?
C9 C10 C11 C12 13(4) . . . . ?
C10 C11 C12 O2 -8(4) . . . . ?
C18 C13 C14 C15 -9(3) . . . . ?
Lu C13 C14 C15 -173.6(16) . . . . ?
C18 C13 C14 P 175.5(14) . . . . ?
Lu C13 C14 P 11(2) . . . . ?
C13 C14 C15 C16 7(3) . . . . ?
P C14 C15 C16 -177.8(17) . . . . ?
C14 C15 C16 C17 0(3) . . . . ?
C15 C16 C17 C18 -3(4) . . . . ?
C16 C17 C18 C13 1(4) . . . . ?
C14 C13 C18 C17 5(3) . . . . ?
Lu C13 C18 C17 167.8(18) . . . . ?
C24 C19 C20 C21 0(3) . . . . ?
P C19 C20 C21 179.3(16) . . . . ?
C19 C20 C21 C22 0(3) . . . . ?
C20 C21 C22 C23 -2(3) . . . . ?
C21 C22 C23 C24 3(3) . . . . ?
C22 C23 C24 C19 -3(3) . . . . ?
C22 C23 C24 Lu -170.1(13) . . . 3_557 ?
C20 C19 C24 C23 1(2) . . . . ?
P C19 C24 C23 -178.1(14) . . . . ?
C20 C19 C24 Lu 170.2(13) . . . 3_557 ?
P C19 C24 Lu -9.2(18) . . . 3_557 ?
C30 C25 C26 C27 3(3) . . . . ?
P C25 C26 C27 -178.4(18) . . . . ?
C25 C26 C27 C28 -2(4) . . . . ?
C26 C27 C28 C29 -1(3) . . . . ?
C27 C28 C29 C30 3(3) . . . . ?
C28 C29 C30 C25 -1(3) . . . . ?
C26 C25 C30 C29 -2(3) . . . . ?
P C25 C30 C29 179.9(17) . . . . ?
C2 C3 O1 C8 179.3(17) . . . . ?
C4 C3 O1 C8 2(3) . . . . ?
C2 C3 O1 Lu -8.4(19) . . . . ?
C4 C3 O1 Lu 174.0(13) . . . . ?
C10 C9 O2 C12 11(4) . . . . ?
C10 C9 O2 Lu -149(2) . . . . ?
C11 C12 O2 C9 -2(3) . . . . ?
C11 C12 O2 Lu 158(2) . . . . ?
C20 C19 P C1 -161.2(15) . . . 3_557 ?
C24 C19 P C1 18.2(16) . . . 3_557 ?
C20 C19 P C14 -37.1(17) . . . . ?
C24 C19 P C14 142.3(14) . . . . ?
C20 C19 P C25 75.1(17) . . . . ?
C24 C19 P C25 -105.5(15) . . . . ?
C20 C19 P Lu -114.4(15) . . . . ?
C24 C19 P Lu 65.0(14) . . . . ?
C15 C14 P C1 -154.3(17) . . . 3_557 ?
C13 C14 P C1 21.5(19) . . . 3_557 ?
C15 C14 P C19 86(2) . . . . ?
C13 C14 P C19 -98.4(16) . . . . ?
C15 C14 P C25 -27(2) . . . . ?
C13 C14 P C25 149.0(16) . . . . ?
C15 C14 P Lu 177(2) . . . . ?
C13 C14 P Lu -7.2(14) . . . . ?
C26 C25 P C1 82.2(19) . . . 3_557 ?
C30 C25 P C1 -99.4(18) . . . 3_557 ?
C26 C25 P C19 -158.8(17) . . . . ?
C30 C25 P C19 19.6(19) . . . . ?
C26 C25 P C14 -45(2) . . . . ?
C30 C25 P C14 133.4(18) . . . . ?
C26 C25 P Lu 46(3) . . . . ?
C30 C25 P Lu -135.6(17) . . . . ?
C2 C1 Lu O2 -75.1(11) . . . . ?
P C1 Lu O2 73.7(9) 3_557 . . . ?
Lu C1 Lu O2 178.8(5) 3_557 . . . ?
C2 C1 Lu C24 -160.5(11) . . . 3_557 ?
P C1 Lu C24 -11.7(8) 3_557 . . 3_557 ?
Lu C1 Lu C24 93.5(6) 3_557 . . 3_557 ?
C2 C1 Lu O1 -2.1(10) . . . . ?
P C1 Lu O1 146.6(9) 3_557 . . . ?
Lu C1 Lu O1 -108.2(6) 3_557 . . . ?
C2 C1 Lu C13 42.4(15) . . . . ?
P C1 Lu C13 -168.8(8) 3_557 . . . ?
Lu C1 Lu C13 -63.7(11) 3_557 . . . ?
C2 C1 Lu C1 106.1(11) . . . 3_557 ?
P C1 Lu C1 -105.2(10) 3_557 . . 3_557 ?
Lu C1 Lu C1 0.0 3_557 . . 3_557 ?
C2 C1 Lu P 79.0(10) . . . . ?
P C1 Lu P -132.3(6) 3_557 . . . ?
Lu C1 Lu P -27.1(5) 3_557 . . . ?
C2 C1 Lu Lu 106.1(11) . . . 3_557 ?
P C1 Lu Lu -105.2(10) 3_557 . . 3_557 ?
C9 O2 Lu C1 26(2) . . . . ?
C12 O2 Lu C1 -131.2(17) . . . . ?
C9 O2 Lu C24 104.8(19) . . . 3_557 ?
C12 O2 Lu C24 -52.0(17) . . . 3_557 ?
C9 O2 Lu O1 -38.3(19) . . . . ?
C12 O2 Lu O1 164.9(17) . . . . ?
C9 O2 Lu C13 -124.1(19) . . . . ?
C12 O2 Lu C13 79.1(17) . . . . ?
C9 O2 Lu C1 -159(2) . . . 3_557 ?
C12 O2 Lu C1 45(3) . . . 3_557 ?
C9 O2 Lu P -111.3(18) . . . . ?
C12 O2 Lu P 91.9(18) . . . . ?
C9 O2 Lu Lu 28(2) . . . 3_557 ?
C12 O2 Lu Lu -129.3(16) . . . 3_557 ?
C3 O1 Lu C1 5.6(11) . . . . ?
C8 O1 Lu C1 177.5(16) . . . . ?
C3 O1 Lu O2 119.7(12) . . . . ?
C8 O1 Lu O2 -68.4(15) . . . . ?
C3 O1 Lu C24 42.0(15) . . . 3_557 ?
C8 O1 Lu C24 -146.1(15) . . . 3_557 ?
C3 O1 Lu C13 -150.8(12) . . . . ?
C8 O1 Lu C13 21.1(15) . . . . ?
C3 O1 Lu C1 -75.2(12) . . . 3_557 ?
C8 O1 Lu C1 96.7(15) . . . 3_557 ?
C3 O1 Lu P -97.4(11) . . . . ?
C8 O1 Lu P 74.5(15) . . . . ?
C3 O1 Lu Lu -37.0(11) . . . 3_557 ?
C8 O1 Lu Lu 134.9(15) . . . 3_557 ?
C14 C13 Lu C1 40(2) . . . . ?
C18 C13 Lu C1 -121.5(17) . . . . ?
C14 C13 Lu O2 163.4(16) . . . . ?
C18 C13 Lu O2 1.4(18) . . . . ?
C14 C13 Lu C24 -109.1(16) . . . 3_557 ?
C18 C13 Lu C24 88.9(19) . . . 3_557 ?
C14 C13 Lu O1 81.2(16) . . . . ?
C18 C13 Lu O1 -80.7(17) . . . . ?
C14 C13 Lu C1 -26.2(15) . . . 3_557 ?
C18 C13 Lu C1 171.9(18) . . . 3_557 ?
C14 C13 Lu P -6.6(13) . . . . ?
C18 C13 Lu P -169(2) . . . . ?
C14 C13 Lu Lu -3.7(17) . . . 3_557 ?
C18 C13 Lu Lu -165.6(16) . . . 3_557 ?
C1 P Lu C1 66.2(10) 3_557 . . . ?
C19 P Lu C1 -43.3(7) . . . . ?
C14 P Lu C1 -150.2(8) . . . . ?
C25 P Lu C1 112.7(18) . . . . ?
C1 P Lu O2 -154.9(10) 3_557 . . . ?
C19 P Lu O2 95.6(9) . . . . ?
C14 P Lu O2 -11.3(10) . . . . ?
C25 P Lu O2 -108.4(18) . . . . ?
C1 P Lu C24 -18.7(9) 3_557 . . 3_557 ?
C19 P Lu C24 -128.2(7) . . . 3_557 ?
C14 P Lu C24 124.9(8) . . . 3_557 ?
C25 P Lu C24 27.8(18) . . . 3_557 ?
C1 P Lu O1 133.3(8) 3_557 . . . ?
C19 P Lu O1 23.8(7) . . . . ?
C14 P Lu O1 -83.1(8) . . . . ?
C25 P Lu O1 179.9(17) . . . . ?
C1 P Lu C13 -138.9(9) 3_557 . . . ?
C19 P Lu C13 111.6(8) . . . . ?
C14 P Lu C13 4.8(9) . . . . ?
C25 P Lu C13 -92.3(18) . . . . ?
C19 P Lu C1 -109.5(9) . . . 3_557 ?
C14 P Lu C1 143.6(10) . . . 3_557 ?
C25 P Lu C1 46.6(18) . . . 3_557 ?
C1 P Lu Lu 44.2(7) 3_557 . . 3_557 ?
C19 P Lu Lu -65.3(6) . . . 3_557 ?
C14 P Lu Lu -172.1(7) . . . 3_557 ?
C25 P Lu Lu 90.8(17) . . . 3_557 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        23.26
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.476
_refine_diff_density_min         -2.770
_refine_diff_density_rms         0.224

#-----------------END

data_ruf7
_database_code_depnum_ccdc_archive 'CCDC 245413'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Triphenylphosphonium-ortho-methoxybenzylide
;
_chemical_name_common            Triphenylphosphonium-ortho-methoxybenzylide
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H23 O P'
_chemical_formula_sum            'C26 H23 O P'
_chemical_formula_weight         382.41

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7457(18)
_cell_length_b                   10.0458(18)
_cell_length_c                   10.715(2)
_cell_angle_alpha                73.76(2)
_cell_angle_beta                 85.61(2)
_cell_angle_gamma                89.94(2)
_cell_volume                     1004.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5000
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      25.0

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    none
_exptl_crystal_F_000             404
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.8942
_exptl_absorpt_correction_T_max  0.9881
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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 IPDS diffractometer'
_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            6420
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.77
_diffrn_reflns_theta_max         25.25
_reflns_number_total             3401
_reflns_number_gt                2577
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (Stoe & Cie, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'

_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^ > 2sigma(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^)+(0.0553P)^2^] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3401
_refine_ls_number_parameters     276
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0937
_refine_ls_wR_factor_gt          0.0889
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_restrained_S_all      0.934
_refine_ls_shift/su_max          0.000
_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 0.4492(2) 0.19969(18) 0.13971(16) 0.0187(4) Uani 1 1 d . . .
C2 C 0.5571(2) 0.1095(2) 0.13482(18) 0.0223(4) Uani 1 1 d . . .
H2 H 0.5378 0.0179 0.1316 0.027 Uiso 1 1 calc R . .
C3 C 0.6921(2) 0.1525(2) 0.13466(19) 0.0282(5) Uani 1 1 d . . .
H3 H 0.7647 0.0898 0.1324 0.034 Uiso 1 1 calc R . .
C4 C 0.7220(2) 0.2860(2) 0.13773(19) 0.0289(5) Uani 1 1 d . . .
H4 H 0.815(3) 0.319(2) 0.136(2) 0.035(6) Uiso 1 1 d . . .
C5 C 0.6153(2) 0.3765(2) 0.14339(19) 0.0288(5) Uani 1 1 d . . .
H5 H 0.6352 0.4682 0.1459 0.031(6) Uiso 1 1 calc R . .
C6 C 0.4796(2) 0.33341(19) 0.14536(18) 0.0233(4) Uani 1 1 d . . .
H6 H 0.4071 0.3953 0.1506 0.028 Uiso 1 1 calc R . .
C7 C 0.24383(19) 0.18908(17) -0.04121(17) 0.0169(4) Uani 1 1 d . . .
C8 C 0.3484(2) 0.23629(18) -0.13874(17) 0.0198(4) Uani 1 1 d . . .
H7 H 0.4397 0.2456 -0.1164 0.024 Uiso 1 1 calc R . .
C9 C 0.3206(2) 0.27040(19) -0.27021(18) 0.0232(4) Uani 1 1 d . . .
H9 H 0.3926 0.3026 -0.3369 0.028 Uiso 1 1 calc R . .
C10 C 0.1868(2) 0.25672(19) -0.30224(18) 0.0250(5) Uani 1 1 d . . .
H10 H 0.1673 0.2811 -0.3912 0.030 Uiso 1 1 calc R . .
C11 C 0.0819(2) 0.2080(2) -0.20578(19) 0.0256(5) Uani 1 1 d . . .
H11 H -0.0089 0.1970 -0.2285 0.031 Uiso 1 1 calc R . .
C12 C 0.1096(2) 0.1749(2) -0.07512(19) 0.0220(4) Uani 1 1 d . . .
H12 H 0.041(2) 0.142(2) -0.009(2) 0.027(6) Uiso 1 1 d . . .
C13 C 0.15741(19) 0.23359(19) 0.20492(18) 0.0201(4) Uani 1 1 d . . .
C14 C 0.0798(2) 0.1715(2) 0.32110(19) 0.0254(5) Uani 1 1 d . . .
H14 H 0.087(2) 0.077(2) 0.357(2) 0.031(6) Uiso 1 1 d . . .
C15 C -0.0060(2) 0.2513(3) 0.3793(2) 0.0348(6) Uani 1 1 d . . .
H15 H -0.058(3) 0.211(3) 0.452(3) 0.048(7) Uiso 1 1 d . . .
C16 C -0.0179(2) 0.3920(3) 0.3210(2) 0.0368(6) Uani 1 1 d . . .
H16 H -0.081(2) 0.445(2) 0.358(2) 0.036(6) Uiso 1 1 d . . .
C17 C 0.0535(2) 0.4533(2) 0.2026(2) 0.0337(5) Uani 1 1 d . . .
H17 H 0.0430 0.5492 0.1611 0.040 Uiso 1 1 calc R . .
C18 C 0.1407(2) 0.37515(19) 0.1442(2) 0.0255(5) Uani 1 1 d . . .
H18 H 0.1894 0.4177 0.0625 0.031 Uiso 1 1 calc R . .
C19 C 0.2595(2) -0.04229(18) 0.17062(17) 0.0199(4) Uani 1 1 d . . .
H19 H 0.2196 -0.0759 0.1068 0.024 Uiso 1 1 calc R . .
C20 C 0.29413(19) -0.15049(18) 0.28468(17) 0.0185(4) Uani 1 1 d . . .
C21 C 0.2900(2) -0.29103(19) 0.2851(2) 0.0246(4) Uani 1 1 d . . .
H21 H 0.2654 -0.3138 0.2093 0.030 Uiso 1 1 calc R . .
C22 C 0.3209(2) -0.3976(2) 0.3939(2) 0.0324(5) Uani 1 1 d . . .
H22 H 0.3165 -0.4914 0.3917 0.039 Uiso 1 1 calc R . .
C23 C 0.3582(2) -0.3666(2) 0.5052(2) 0.0306(5) Uani 1 1 d . . .
H23 H 0.3799 -0.4389 0.5791 0.037 Uiso 1 1 calc R . .
C24 C 0.3635(2) -0.2297(2) 0.50819(18) 0.0261(5) Uani 1 1 d . . .
H24 H 0.3882 -0.2081 0.5845 0.031 Uiso 1 1 calc R . .
C25 C 0.33282(19) -0.12386(18) 0.39979(17) 0.0198(4) Uani 1 1 d . . .
C26 C 0.3220(2) 0.0500(2) 0.51545(19) 0.0302(5) Uani 1 1 d . . .
H26A H 0.4015 0.0172 0.5654 0.036 Uiso 1 1 calc R . .
H26B H 0.2377 0.0060 0.5658 0.036 Uiso 1 1 calc R . .
H26C H 0.3165 0.1509 0.4980 0.036 Uiso 1 1 calc R . .
P P 0.27696(5) 0.13251(5) 0.13018(4) 0.01640(15) Uani 1 1 d . . .
O O 0.33689(15) 0.01501(13) 0.39495(12) 0.0240(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0229(11) 0.0210(9) 0.0115(8) -0.0028(7) -0.0034(8) 0.0004(8)
C2 0.0231(11) 0.0253(10) 0.0210(9) -0.0103(8) -0.0028(9) 0.0018(9)
C3 0.0229(11) 0.0417(12) 0.0227(10) -0.0127(9) -0.0048(9) 0.0053(10)
C4 0.0224(12) 0.0439(12) 0.0182(10) -0.0043(9) -0.0033(9) -0.0086(10)
C5 0.0359(13) 0.0268(10) 0.0227(10) -0.0045(8) -0.0043(10) -0.0116(10)
C6 0.0268(11) 0.0221(9) 0.0206(9) -0.0043(8) -0.0046(8) -0.0005(8)
C7 0.0193(10) 0.0148(8) 0.0168(9) -0.0047(7) -0.0019(8) 0.0025(8)
C8 0.0220(11) 0.0184(9) 0.0191(9) -0.0053(7) -0.0028(8) 0.0006(8)
C9 0.0287(12) 0.0230(9) 0.0171(9) -0.0049(8) 0.0015(9) 0.0005(9)
C10 0.0325(12) 0.0269(10) 0.0175(9) -0.0077(8) -0.0071(9) 0.0072(9)
C11 0.0244(11) 0.0297(10) 0.0254(10) -0.0103(9) -0.0095(9) 0.0067(9)
C12 0.0194(11) 0.0253(10) 0.0202(10) -0.0053(8) 0.0003(9) 0.0005(9)
C13 0.0168(10) 0.0257(10) 0.0198(9) -0.0093(8) -0.0027(8) 0.0013(8)
C14 0.0189(11) 0.0340(11) 0.0224(10) -0.0063(9) -0.0017(9) 0.0001(9)
C15 0.0179(12) 0.0627(16) 0.0267(11) -0.0183(11) 0.0025(10) 0.0014(11)
C16 0.0208(12) 0.0532(14) 0.0496(14) -0.0356(12) -0.0040(11) 0.0089(11)
C17 0.0259(12) 0.0295(11) 0.0521(14) -0.0212(11) -0.0060(11) 0.0038(10)
C18 0.0228(11) 0.0231(10) 0.0311(10) -0.0089(8) 0.0000(9) 0.0004(9)
C19 0.0224(11) 0.0205(9) 0.0175(9) -0.0057(7) -0.0054(8) -0.0013(8)
C20 0.0135(10) 0.0206(9) 0.0187(9) -0.0018(8) 0.0018(8) -0.0010(8)
C21 0.0211(11) 0.0221(9) 0.0301(10) -0.0061(8) -0.0025(9) -0.0011(8)
C22 0.0287(13) 0.0190(9) 0.0437(13) -0.0005(9) 0.0014(10) 0.0003(9)
C23 0.0279(12) 0.0290(11) 0.0257(10) 0.0066(9) -0.0002(9) 0.0042(9)
C24 0.0216(11) 0.0346(11) 0.0170(9) 0.0007(8) 0.0001(8) 0.0039(9)
C25 0.0160(10) 0.0214(9) 0.0193(9) -0.0025(8) 0.0021(8) 0.0002(8)
C26 0.0310(13) 0.0422(12) 0.0233(10) -0.0183(9) -0.0041(9) 0.0039(10)
P 0.0179(3) 0.0173(2) 0.0138(2) -0.00404(18) -0.00121(19) 0.00027(19)
O 0.0327(8) 0.0251(7) 0.0157(6) -0.0080(5) -0.0035(6) 0.0026(6)

_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 1.394(3) . ?
C1 C6 1.395(3) . ?
C1 P 1.831(2) . ?
C2 C3 1.385(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(3) . ?
C4 H4 0.97(2) . ?
C5 C6 1.388(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.385(3) . ?
C7 C12 1.402(3) . ?
C7 P 1.8184(17) . ?
C8 C9 1.401(2) . ?
C8 H7 0.9500 . ?
C9 C10 1.390(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.93(2) . ?
C13 C14 1.391(3) . ?
C13 C18 1.404(3) . ?
C13 P 1.8273(19) . ?
C14 C15 1.389(3) . ?
C14 H14 0.93(2) . ?
C15 C16 1.385(3) . ?
C15 H15 0.89(3) . ?
C16 C17 1.379(3) . ?
C16 H16 0.95(2) . ?
C17 C18 1.386(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.452(2) . ?
C19 P 1.6925(18) . ?
C19 H19 0.9500 . ?
C20 C25 1.411(3) . ?
C20 C21 1.411(3) . ?
C21 C22 1.397(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.388(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.386(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(2) . ?
C24 H24 0.9500 . ?
C25 O 1.382(2) . ?
C26 O 1.427(2) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

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 C6 118.88(19) . . ?
C2 C1 P 115.85(14) . . ?
C6 C1 P 125.20(14) . . ?
C3 C2 C1 120.50(18) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 120.46(19) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.6(2) . . ?
C3 C4 H4 121.9(13) . . ?
C5 C4 H4 118.5(13) . . ?
C6 C5 C4 120.23(19) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 120.36(18) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
C8 C7 C12 119.39(16) . . ?
C8 C7 P 121.97(14) . . ?
C12 C7 P 118.49(15) . . ?
C7 C8 C9 120.44(18) . . ?
C7 C8 H7 119.8 . . ?
C9 C8 H7 119.8 . . ?
C10 C9 C8 119.48(19) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 120.59(17) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 119.83(19) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C7 120.3(2) . . ?
C11 C12 H12 121.2(13) . . ?
C7 C12 H12 118.5(13) . . ?
C14 C13 C18 118.90(18) . . ?
C14 C13 P 120.82(14) . . ?
C18 C13 P 120.27(15) . . ?
C15 C14 C13 119.9(2) . . ?
C15 C14 H14 122.1(14) . . ?
C13 C14 H14 118.0(14) . . ?
C16 C15 C14 120.6(2) . . ?
C16 C15 H15 119.2(16) . . ?
C14 C15 H15 120.1(16) . . ?
C17 C16 C15 119.9(2) . . ?
C17 C16 H16 119.5(14) . . ?
C15 C16 H16 120.4(14) . . ?
C16 C17 C18 120.0(2) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C13 120.5(2) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C20 C19 P 131.98(14) . . ?
C20 C19 H19 114.0 . . ?
P C19 H19 114.0 . . ?
C25 C20 C21 116.18(15) . . ?
C25 C20 C19 123.38(16) . . ?
C21 C20 C19 120.44(17) . . ?
C22 C21 C20 121.80(18) . . ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
C23 C22 C21 120.04(19) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 119.71(17) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 120.14(18) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
O C25 C24 123.51(17) . . ?
O C25 C20 114.36(14) . . ?
C24 C25 C20 122.13(17) . . ?
O C26 H26A 109.5 . . ?
O C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 P C7 104.19(9) . . ?
C19 P C13 120.19(10) . . ?
C7 P C13 103.38(8) . . ?
C19 P C1 115.70(9) . . ?
C7 P C1 105.93(9) . . ?
C13 P C1 105.86(9) . . ?
C25 O C26 117.83(15) . . ?

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
C6 C1 C2 C3 -0.4(3) . . . . ?
P C1 C2 C3 176.73(14) . . . . ?
C1 C2 C3 C4 -0.8(3) . . . . ?
C2 C3 C4 C5 1.2(3) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C4 C5 C6 C1 -1.0(3) . . . . ?
C2 C1 C6 C5 1.3(3) . . . . ?
P C1 C6 C5 -175.58(14) . . . . ?
C12 C7 C8 C9 0.3(3) . . . . ?
P C7 C8 C9 175.76(13) . . . . ?
C7 C8 C9 C10 0.1(3) . . . . ?
C8 C9 C10 C11 -1.0(3) . . . . ?
C9 C10 C11 C12 1.3(3) . . . . ?
C10 C11 C12 C7 -0.9(3) . . . . ?
C8 C7 C12 C11 0.0(3) . . . . ?
P C7 C12 C11 -175.54(14) . . . . ?
C18 C13 C14 C15 -4.0(3) . . . . ?
P C13 C14 C15 177.20(16) . . . . ?
C13 C14 C15 C16 1.6(3) . . . . ?
C14 C15 C16 C17 1.5(3) . . . . ?
C15 C16 C17 C18 -2.2(3) . . . . ?
C16 C17 C18 C13 -0.2(3) . . . . ?
C14 C13 C18 C17 3.3(3) . . . . ?
P C13 C18 C17 -177.87(15) . . . . ?
P C19 C20 C25 10.8(3) . . . . ?
P C19 C20 C21 -169.36(17) . . . . ?
C25 C20 C21 C22 0.7(3) . . . . ?
C19 C20 C21 C22 -179.12(19) . . . . ?
C20 C21 C22 C23 -0.6(3) . . . . ?
C21 C22 C23 C24 0.5(3) . . . . ?
C22 C23 C24 C25 -0.5(3) . . . . ?
C23 C24 C25 O -179.49(19) . . . . ?
C23 C24 C25 C20 0.7(3) . . . . ?
C21 C20 C25 O 179.41(17) . . . . ?
C19 C20 C25 O -0.8(3) . . . . ?
C21 C20 C25 C24 -0.8(3) . . . . ?
C19 C20 C25 C24 179.04(19) . . . . ?
C20 C19 P C7 168.23(19) . . . . ?
C20 C19 P C13 -76.7(2) . . . . ?
C20 C19 P C1 52.4(2) . . . . ?
C8 C7 P C19 -106.24(16) . . . . ?
C12 C7 P C19 69.21(15) . . . . ?
C8 C7 P C13 127.37(15) . . . . ?
C12 C7 P C13 -57.18(16) . . . . ?
C8 C7 P C1 16.26(16) . . . . ?
C12 C7 P C1 -168.29(14) . . . . ?
C14 C13 P C19 19.90(19) . . . . ?
C18 C13 P C19 -158.88(15) . . . . ?
C14 C13 P C7 135.36(16) . . . . ?
C18 C13 P C7 -43.42(18) . . . . ?
C14 C13 P C1 -113.49(16) . . . . ?
C18 C13 P C1 67.74(17) . . . . ?
C2 C1 P C19 21.12(17) . . . . ?
C6 C1 P C19 -161.90(15) . . . . ?
C2 C1 P C7 -93.73(15) . . . . ?
C6 C1 P C7 83.24(16) . . . . ?
C2 C1 P C13 156.92(14) . . . . ?
C6 C1 P C13 -26.10(18) . . . . ?
C24 C25 O C26 -23.5(3) . . . . ?
C20 C25 O C26 156.30(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.937
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.937
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.050


#-------------------------------------------------------------------------

data_ks394
_database_code_depnum_ccdc_archive 'CCDC 286123'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H72 O6 P2 Y2'
_chemical_formula_weight         1225.02

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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.513(3)
_cell_length_b                   14.455(3)
_cell_length_c                   19.023(4)
_cell_angle_alpha                86.89(3)
_cell_angle_beta                 75.64(3)
_cell_angle_gamma                70.68(3)
_cell_volume                     3144.4(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    all
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    1.936
_exptl_absorpt_correction_type   'mean imaging plate intensity method'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(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-IPDSII
_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            40601
_diffrn_reflns_av_R_equivalents  0.1327
_diffrn_reflns_av_sigmaI/netI    0.1414
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11055
_reflns_number_gt                6310
_reflns_threshold_expression     >2sigma(I)

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

_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^ > 2sigma(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^)+(0.0682P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         11055
_refine_ls_number_parameters     667
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1511
_refine_ls_wR_factor_gt          0.1338
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_restrained_S_all      0.897
_refine_ls_shift/su_max          0.000
_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
C28A C -0.243(2) 0.8530(19) 0.3829(12) 0.179(15) Uiso 0.59(2) 1 d PD A 1
H28A H -0.2086 0.7857 0.3612 0.215 Uiso 0.59(2) 1 calc PR A 1
H28B H -0.3240 0.8828 0.3785 0.215 Uiso 0.59(2) 1 calc PR A 1
C29A C -0.2313(9) 0.857(2) 0.4637(12) 0.120(10) Uiso 0.59(2) 1 d PD A 1
H29A H -0.2692 0.9237 0.4861 0.144 Uiso 0.59(2) 1 calc PR A 1
H29B H -0.2621 0.8098 0.4948 0.144 Uiso 0.59(2) 1 calc PR A 1
C28B C -0.2631(16) 0.9334(12) 0.4243(8) 0.066(8) Uiso 0.41(2) 1 d PD A 2
H28C H -0.3428 0.9542 0.4162 0.079 Uiso 0.41(2) 1 calc PR A 2
H28D H -0.2584 0.9781 0.4602 0.079 Uiso 0.41(2) 1 calc PR A 2
C29B C -0.2178(13) 0.8216(15) 0.4438(17) 0.075(9) Uiso 0.41(2) 1 d PD A 2
H29C H -0.2623 0.8069 0.4913 0.090 Uiso 0.41(2) 1 calc PR A 2
H29D H -0.2145 0.7765 0.4054 0.090 Uiso 0.41(2) 1 calc PR A 2
C58A C 0.7641(7) 0.4492(13) 0.2929(8) 0.048(5) Uiso 0.49(2) 1 d PD B 1
H58A H 0.8080 0.3796 0.2786 0.058 Uiso 0.49(2) 1 calc PR B 1
H58B H 0.7648 0.4624 0.3433 0.058 Uiso 0.49(2) 1 calc PR B 1
C59A C 0.8041(11) 0.5193(9) 0.2396(9) 0.058(6) Uiso 0.49(2) 1 d PD B 1
H59A H 0.8452 0.4837 0.1924 0.070 Uiso 0.49(2) 1 calc PR B 1
H59B H 0.8613 0.5397 0.2571 0.070 Uiso 0.49(2) 1 calc PR B 1
C58B C 0.7580(10) 0.4856(13) 0.2891(11) 0.069(6) Uiso 0.51(2) 1 d PD B 2
H58C H 0.7677 0.4590 0.3371 0.083 Uiso 0.51(2) 1 calc PR B 2
H58D H 0.8206 0.4404 0.2518 0.083 Uiso 0.51(2) 1 calc PR B 2
C59B C 0.7786(17) 0.5832(12) 0.2838(9) 0.076(7) Uiso 0.51(2) 1 d PD B 2
H59C H 0.7423 0.6246 0.3288 0.092 Uiso 0.51(2) 1 calc PR B 2
H59D H 0.8616 0.5783 0.2653 0.092 Uiso 0.51(2) 1 calc PR B 2
Y1 Y 0.12680(5) 0.82513(4) 0.29414(3) 0.02718(18) Uani 1 1 d . . .
Y2 Y 0.42167(5) 0.66244(4) 0.22004(3) 0.02237(16) Uani 1 1 d . . .
P1 P 0.34006(16) 0.92052(12) 0.23872(9) 0.0303(4) Uani 1 1 d . . .
P2 P 0.18851(15) 0.57541(12) 0.27278(8) 0.0279(4) Uani 1 1 d . . .
O1 O 0.1728(4) 0.7993(3) 0.4121(2) 0.0348(11) Uani 1 1 d . . .
O2 O 0.3288(4) 0.6860(3) 0.1108(2) 0.0279(10) Uani 1 1 d . . .
O3 O -0.0621(4) 0.8704(4) 0.3786(3) 0.0521(14) Uani 1 1 d . A .
O4 O 0.6152(4) 0.5692(4) 0.2380(3) 0.0424(12) Uani 1 1 d . B .
O5 O 0.5694(4) 0.6579(3) 0.1055(2) 0.0358(11) Uani 1 1 d . . .
C1 C 0.3080(5) 0.8322(4) 0.2009(3) 0.0250(14) Uani 1 1 d . . .
C2 C 0.2505(5) 0.8557(4) 0.1417(3) 0.0281(14) Uani 1 1 d . . .
C3 C 0.2595(6) 0.7782(5) 0.0941(3) 0.0315(15) Uani 1 1 d . . .
C4 C 0.2083(6) 0.7925(5) 0.0379(4) 0.0405(17) Uani 1 1 d . . .
H4 H 0.2194 0.7382 0.0077 0.049 Uiso 1 1 calc R . .
C5 C 0.1391(7) 0.8864(6) 0.0235(4) 0.055(2) Uani 1 1 d . . .
H5 H 0.1023 0.8964 -0.0157 0.065 Uiso 1 1 calc R . .
C6 C 0.1260(7) 0.9637(6) 0.0679(4) 0.054(2) Uani 1 1 d . . .
H6 H 0.0799 1.0281 0.0591 0.065 Uiso 1 1 calc R . .
C7 C 0.1791(6) 0.9485(5) 0.1250(4) 0.0423(18) Uani 1 1 d . . .
H7 H 0.1670 1.0034 0.1548 0.051 Uiso 1 1 calc R . .
C8 C 0.4521(6) 0.9659(5) 0.1789(4) 0.0369(17) Uani 1 1 d . . .
C9 C 0.5666(7) 0.9327(6) 0.1844(4) 0.053(2) Uani 1 1 d . . .
H9 H 0.5875 0.8889 0.2215 0.063 Uiso 1 1 calc R . .
C10 C 0.6509(8) 0.9621(7) 0.1365(5) 0.069(3) Uani 1 1 d . . .
H10 H 0.7290 0.9402 0.1415 0.083 Uiso 1 1 calc R . .
C11 C 0.6215(9) 1.0230(7) 0.0821(6) 0.079(3) Uani 1 1 d . . .
H11 H 0.6795 1.0432 0.0491 0.094 Uiso 1 1 calc R . .
C12 C 0.5108(9) 1.0547(6) 0.0747(5) 0.068(3) Uani 1 1 d . . .
H12 H 0.4924 1.0963 0.0360 0.082 Uiso 1 1 calc R . .
C13 C 0.4222(7) 1.0277(5) 0.1229(4) 0.053(2) Uani 1 1 d . . .
H13 H 0.3443 1.0508 0.1176 0.064 Uiso 1 1 calc R . .
C14 C 0.2163(6) 1.0272(5) 0.2764(3) 0.0361(17) Uani 1 1 d . . .
C15 C 0.1134(6) 1.0048(5) 0.3065(3) 0.0364(16) Uani 1 1 d . . .
C16 C 0.0176(7) 1.0861(5) 0.3403(4) 0.0448(19) Uani 1 1 d . . .
H16 H -0.0539 1.0756 0.3633 0.054 Uiso 1 1 calc R . .
C17 C 0.0226(8) 1.1790(5) 0.3416(4) 0.059(2) Uani 1 1 d . . .
H17 H -0.0454 1.2311 0.3639 0.070 Uiso 1 1 calc R . .
C18 C 0.1249(8) 1.1982(6) 0.3110(5) 0.066(3) Uani 1 1 d . . .
H18 H 0.1277 1.2629 0.3126 0.080 Uiso 1 1 calc R . .
C19 C 0.2235(7) 1.1221(5) 0.2779(4) 0.051(2) Uani 1 1 d . . .
H19 H 0.2948 1.1338 0.2565 0.061 Uiso 1 1 calc R . .
C20 C 0.4026(6) 0.8674(5) 0.3136(3) 0.0347(16) Uani 1 1 d . . .
C21 C 0.4445(6) 0.7633(5) 0.3159(3) 0.0321(15) Uani 1 1 d . . .
C22 C 0.4918(6) 0.7288(6) 0.3746(4) 0.0436(18) Uani 1 1 d . . .
H22 H 0.5183 0.6599 0.3802 0.052 Uiso 1 1 calc R . .
C23 C 0.5032(7) 0.7872(7) 0.4255(4) 0.051(2) Uani 1 1 d . . .
H23 H 0.5396 0.7584 0.4633 0.061 Uiso 1 1 calc R . .
C24 C 0.4607(8) 0.8887(7) 0.4206(4) 0.060(2) Uani 1 1 d . . .
H24 H 0.4667 0.9300 0.4556 0.072 Uiso 1 1 calc R . .
C25 C 0.4100(7) 0.9288(6) 0.3647(4) 0.0459(19) Uani 1 1 d . . .
H25 H 0.3802 0.9979 0.3611 0.055 Uiso 1 1 calc R . .
C26 C 0.3500(7) 0.6073(5) 0.0601(3) 0.0383(17) Uani 1 1 d . . .
H26A H 0.3997 0.5460 0.0758 0.057 Uiso 1 1 calc R . .
H26B H 0.3892 0.6224 0.0117 0.057 Uiso 1 1 calc R . .
H26C H 0.2755 0.6002 0.0584 0.057 Uiso 1 1 calc R . .
C27 C -0.1645(7) 0.9195(8) 0.3514(6) 0.079(3) Uani 1 1 d D . .
H27A H -0.1453 0.9190 0.2977 0.095 Uiso 1 1 calc R A 1
H27B H -0.2029 0.9880 0.3705 0.095 Uiso 1 1 calc R A 1
C30 C -0.0934(7) 0.8248(8) 0.4458(5) 0.078(3) Uani 1 1 d D . .
H30A H -0.0674 0.8482 0.4845 0.094 Uiso 1 1 calc R A 1
H30B H -0.0581 0.7525 0.4405 0.094 Uiso 1 1 calc R A 1
C31 C 0.2328(5) 0.6572(4) 0.3104(3) 0.0252(14) Uani 1 1 d . . .
C32 C 0.2682(5) 0.6318(5) 0.3781(3) 0.0263(14) Uani 1 1 d . . .
C33 C 0.2376(6) 0.7066(5) 0.4318(3) 0.0314(15) Uani 1 1 d . . .
C34 C 0.2682(6) 0.6900(6) 0.4962(3) 0.0407(18) Uani 1 1 d . . .
H34 H 0.2444 0.7425 0.5307 0.049 Uiso 1 1 calc R . .
C35 C 0.3338(7) 0.5973(7) 0.5120(4) 0.051(2) Uani 1 1 d . . .
H35 H 0.3566 0.5864 0.5566 0.062 Uiso 1 1 calc R . .
C36 C 0.3657(7) 0.5215(6) 0.4629(4) 0.049(2) Uani 1 1 d . . .
H36 H 0.4095 0.4574 0.4739 0.059 Uiso 1 1 calc R . .
C37 C 0.3338(6) 0.5380(5) 0.3961(4) 0.0365(17) Uani 1 1 d . . .
H37 H 0.3570 0.4846 0.3625 0.044 Uiso 1 1 calc R . .
C38 C 0.0952(7) 0.5207(6) 0.3390(3) 0.0419(19) Uani 1 1 d . . .
C39 C -0.0249(7) 0.5743(7) 0.3618(4) 0.056(2) Uani 1 1 d . . .
H39 H -0.0558 0.6357 0.3411 0.067 Uiso 1 1 calc R . .
C40 C -0.0981(9) 0.5377(9) 0.4142(4) 0.075(3) Uani 1 1 d . . .
H40 H -0.1793 0.5735 0.4284 0.090 Uiso 1 1 calc R . .
C41 C -0.0540(11) 0.4502(9) 0.4455(5) 0.083(4) Uani 1 1 d . . .
H41 H -0.1044 0.4257 0.4817 0.100 Uiso 1 1 calc R . .
C42 C 0.0637(11) 0.3980(7) 0.4245(4) 0.073(3) Uani 1 1 d . . .
H42 H 0.0941 0.3377 0.4466 0.087 Uiso 1 1 calc R . .
C43 C 0.1388(8) 0.4328(6) 0.3710(4) 0.055(2) Uani 1 1 d . . .
H43 H 0.2196 0.3961 0.3567 0.066 Uiso 1 1 calc R . .
C44 C 0.3077(6) 0.4727(4) 0.2225(3) 0.0308(15) Uani 1 1 d . . .
C45 C 0.4152(6) 0.4897(4) 0.2013(3) 0.0293(15) Uani 1 1 d . . .
C46 C 0.5069(7) 0.4092(5) 0.1609(3) 0.0379(17) Uani 1 1 d . . .
H46 H 0.5823 0.4151 0.1441 0.045 Uiso 1 1 calc R . .
C47 C 0.4915(7) 0.3232(5) 0.1451(4) 0.0458(19) Uani 1 1 d . . .
H47 H 0.5563 0.2716 0.1187 0.055 Uiso 1 1 calc R . .
C48 C 0.3840(8) 0.3109(5) 0.1668(4) 0.049(2) Uani 1 1 d . . .
H48 H 0.3738 0.2519 0.1548 0.059 Uiso 1 1 calc R . .
C49 C 0.2910(7) 0.3856(5) 0.2061(4) 0.0397(17) Uani 1 1 d . . .
H49 H 0.2162 0.3781 0.2221 0.048 Uiso 1 1 calc R . .
C50 C 0.0978(5) 0.6396(5) 0.2123(3) 0.0331(16) Uani 1 1 d . . .
C51 C 0.0480(6) 0.7415(5) 0.2190(4) 0.0378(16) Uani 1 1 d . . .
C52 C -0.0267(7) 0.7842(6) 0.1745(4) 0.051(2) Uani 1 1 d . . .
H52 H -0.0617 0.8535 0.1767 0.061 Uiso 1 1 calc R . .
C53 C -0.0530(7) 0.7291(8) 0.1263(4) 0.062(2) Uani 1 1 d . . .
H53 H -0.1056 0.7610 0.0972 0.074 Uiso 1 1 calc R . .
C54 C -0.0023(7) 0.6298(7) 0.1216(4) 0.055(2) Uani 1 1 d . . .
H54 H -0.0192 0.5923 0.0889 0.065 Uiso 1 1 calc R . .
C55 C 0.0732(6) 0.5835(6) 0.1641(4) 0.0423(18) Uani 1 1 d . . .
H55 H 0.1084 0.5142 0.1609 0.051 Uiso 1 1 calc R . .
C56 C 0.1499(8) 0.8797(6) 0.4618(4) 0.056(2) Uani 1 1 d . . .
H56A H 0.1040 0.9408 0.4436 0.084 Uiso 1 1 calc R . .
H56B H 0.2241 0.8853 0.4659 0.084 Uiso 1 1 calc R . .
H56C H 0.1061 0.8673 0.5097 0.084 Uiso 1 1 calc R . .
C57 C 0.6426(6) 0.4822(6) 0.2805(4) 0.053(2) Uani 1 1 d D . .
H57A H 0.6331 0.4281 0.2557 0.064 Uiso 1 1 calc R B 1
H57B H 0.5854 0.4949 0.3283 0.064 Uiso 1 1 calc R B 1
C60 C 0.7088(7) 0.6104(7) 0.2270(5) 0.066(3) Uani 1 1 d D . .
H60A H 0.6914 0.6638 0.2628 0.079 Uiso 1 1 calc R B 1
H60B H 0.7276 0.6343 0.1772 0.079 Uiso 1 1 calc R B 1
C61 C 0.6563(7) 0.5732(5) 0.0635(4) 0.0477(19) Uani 1 1 d . . .
H61A H 0.6196 0.5409 0.0365 0.057 Uiso 1 1 calc R . .
H61B H 0.6958 0.5250 0.0957 0.057 Uiso 1 1 calc R . .
C62 C 0.7428(7) 0.6136(6) 0.0114(5) 0.064(3) Uani 1 1 d . . .
H62A H 0.8181 0.5939 0.0255 0.077 Uiso 1 1 calc R . .
H62B H 0.7570 0.5893 -0.0388 0.077 Uiso 1 1 calc R . .
C63 C 0.6868(7) 0.7229(6) 0.0172(4) 0.054(2) Uani 1 1 d . . .
H63A H 0.6913 0.7512 -0.0316 0.065 Uiso 1 1 calc R . .
H63B H 0.7255 0.7529 0.0445 0.065 Uiso 1 1 calc R . .
C64 C 0.5612(4) 0.7397(3) 0.0574(2) 0.0424(18) Uani 1 1 d . . .
H64A H 0.5275 0.8030 0.0852 0.051 Uiso 1 1 calc R . .
H64B H 0.5129 0.7390 0.0235 0.051 Uiso 1 1 calc R . .
O6 O 0.8440(4) 0.3351(3) 0.1025(2) 0.078(4) Uiso 0.514(7) 1 d PR . .
C65 C 0.8378(4) 0.2578(3) 0.1510(2) 0.066(5) Uiso 0.514(7) 1 d PR . .
H65A H 0.8130 0.2098 0.1296 0.079 Uiso 0.514(7) 1 calc PR . .
H65B H 0.7803 0.2841 0.1973 0.079 Uiso 0.514(7) 1 calc PR . .
C66 C 0.9504(4) 0.2117(3) 0.1636(2) 0.082(6) Uiso 0.514(7) 1 d PR . .
H66A H 0.9468 0.2159 0.2160 0.099 Uiso 0.514(7) 1 calc PR . .
H66B H 0.9796 0.1416 0.1482 0.099 Uiso 0.514(7) 1 calc PR . .
C67 C 1.0262(4) 0.2605(3) 0.1229(2) 0.137(10) Uiso 0.514(7) 1 d PR . .
H67A H 1.0917 0.2138 0.0881 0.164 Uiso 0.514(7) 1 calc PR . .
H67B H 1.0589 0.2881 0.1558 0.164 Uiso 0.514(7) 1 calc PR . .
C68 C 0.9605(4) 0.3368(3) 0.0852(2) 0.097(7) Uiso 0.514(7) 1 d PR . .
H68A H 0.9617 0.4010 0.0999 0.116 Uiso 0.514(7) 1 calc PR . .
H68B H 0.9944 0.3266 0.0322 0.116 Uiso 0.514(7) 1 calc PR . .
O7 O 0.5625(4) 0.1243(3) 0.2979(2) 0.126(7) Uiso 0.486(7) 1 d PR . .
C69 C 0.6707(4) 0.1385(3) 0.2942(2) 0.083(6) Uiso 0.486(7) 1 d PR . .
H69A H 0.7227 0.0814 0.3141 0.100 Uiso 0.486(7) 1 calc PR . .
H69B H 0.7098 0.1455 0.2431 0.100 Uiso 0.486(7) 1 calc PR . .
C70 C 0.6477(4) 0.2248(3) 0.3356(2) 0.085(6) Uiso 0.486(7) 1 d PR . .
H70A H 0.6757 0.2733 0.3043 0.102 Uiso 0.486(7) 1 calc PR . .
H70B H 0.6886 0.2091 0.3753 0.102 Uiso 0.486(7) 1 calc PR . .
C71 C 0.5252(4) 0.2640(3) 0.3648(2) 0.085(6) Uiso 0.486(7) 1 d PR . .
H71A H 0.5074 0.2671 0.4185 0.102 Uiso 0.486(7) 1 calc PR . .
H71B H 0.4945 0.3312 0.3476 0.102 Uiso 0.486(7) 1 calc PR . .
C72 C 0.4725(4) 0.2019(3) 0.3415(2) 0.103(8) Uiso 0.486(7) 1 d PR . .
H72A H 0.4166 0.2393 0.3131 0.123 Uiso 0.486(7) 1 calc PR . .
H72B H 0.4296 0.1752 0.3840 0.123 Uiso 0.486(7) 1 calc PR . .

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
Y1 0.0231(4) 0.0275(4) 0.0280(3) -0.0002(3) 0.0023(3) -0.0105(3)
Y2 0.0226(4) 0.0225(3) 0.0220(3) 0.0019(2) -0.0012(2) -0.0108(3)
P1 0.0340(10) 0.0267(9) 0.0283(8) -0.0021(7) 0.0055(7) -0.0165(8)
P2 0.0308(10) 0.0333(10) 0.0238(8) -0.0009(7) 0.0012(7) -0.0216(8)
O1 0.040(3) 0.039(3) 0.025(2) -0.0061(19) 0.000(2) -0.018(2)
O2 0.033(3) 0.024(2) 0.026(2) -0.0043(17) -0.0034(19) -0.011(2)
O3 0.029(3) 0.056(3) 0.057(3) 0.005(3) 0.011(2) -0.010(3)
O4 0.025(3) 0.052(3) 0.053(3) 0.007(2) -0.011(2) -0.015(2)
O5 0.036(3) 0.034(3) 0.030(2) -0.0011(19) 0.005(2) -0.011(2)
C1 0.026(4) 0.023(3) 0.024(3) -0.003(2) 0.002(3) -0.011(3)
C2 0.025(4) 0.025(3) 0.029(3) 0.002(3) 0.003(3) -0.008(3)
C3 0.025(4) 0.030(4) 0.036(4) 0.003(3) -0.002(3) -0.008(3)
C4 0.042(4) 0.050(5) 0.034(4) 0.000(3) -0.014(3) -0.018(4)
C5 0.043(5) 0.066(6) 0.050(5) 0.011(4) -0.024(4) -0.003(4)
C6 0.042(5) 0.051(5) 0.055(5) 0.007(4) -0.014(4) 0.003(4)
C7 0.039(4) 0.034(4) 0.041(4) 0.000(3) -0.004(3) 0.000(3)
C8 0.045(5) 0.022(3) 0.038(4) -0.006(3) 0.010(3) -0.016(3)
C9 0.049(5) 0.050(5) 0.058(5) -0.001(4) 0.005(4) -0.027(4)
C10 0.052(6) 0.075(7) 0.079(6) -0.006(5) 0.011(5) -0.036(5)
C11 0.066(7) 0.047(5) 0.095(8) -0.013(5) 0.047(6) -0.029(5)
C12 0.087(8) 0.037(5) 0.056(5) 0.011(4) 0.023(5) -0.018(5)
C13 0.056(5) 0.034(4) 0.052(5) 0.005(3) 0.013(4) -0.011(4)
C14 0.046(4) 0.027(4) 0.030(3) -0.004(3) 0.008(3) -0.019(3)
C15 0.038(4) 0.032(4) 0.034(4) -0.003(3) 0.003(3) -0.013(3)
C16 0.046(5) 0.038(4) 0.038(4) -0.006(3) 0.012(3) -0.013(4)
C17 0.065(6) 0.032(4) 0.054(5) -0.017(4) 0.017(4) -0.004(4)
C18 0.083(7) 0.027(4) 0.064(5) -0.012(4) 0.029(5) -0.016(4)
C19 0.063(6) 0.039(4) 0.046(4) -0.009(3) 0.016(4) -0.030(4)
C20 0.036(4) 0.040(4) 0.029(3) -0.003(3) 0.009(3) -0.024(3)
C21 0.030(4) 0.039(4) 0.033(3) 0.001(3) 0.000(3) -0.022(3)
C22 0.041(4) 0.062(5) 0.033(4) 0.002(3) 0.002(3) -0.032(4)
C23 0.054(5) 0.076(6) 0.034(4) 0.004(4) -0.016(4) -0.034(5)
C24 0.066(6) 0.091(7) 0.038(4) -0.020(4) -0.003(4) -0.050(5)
C25 0.056(5) 0.049(5) 0.040(4) -0.014(3) -0.002(4) -0.031(4)
C26 0.054(5) 0.034(4) 0.024(3) -0.005(3) 0.000(3) -0.017(3)
C27 0.035(5) 0.089(8) 0.088(7) -0.012(6) 0.003(5) 0.004(5)
C30 0.053(6) 0.090(7) 0.082(7) 0.019(6) 0.014(5) -0.037(5)
C31 0.026(4) 0.026(3) 0.028(3) 0.007(3) 0.000(3) -0.018(3)
C32 0.020(3) 0.035(4) 0.023(3) 0.004(3) 0.004(2) -0.015(3)
C33 0.025(4) 0.048(4) 0.028(3) 0.000(3) 0.001(3) -0.024(3)
C34 0.040(4) 0.067(5) 0.023(3) 0.000(3) -0.002(3) -0.032(4)
C35 0.045(5) 0.086(7) 0.026(4) 0.008(4) -0.011(3) -0.025(5)
C36 0.038(4) 0.065(5) 0.044(4) 0.023(4) -0.012(3) -0.018(4)
C37 0.037(4) 0.043(4) 0.031(4) 0.008(3) -0.004(3) -0.018(3)
C38 0.054(5) 0.058(5) 0.026(3) -0.010(3) 0.006(3) -0.045(4)
C39 0.055(5) 0.089(6) 0.038(4) -0.011(4) 0.009(4) -0.053(5)
C40 0.076(7) 0.123(9) 0.042(5) -0.017(5) 0.019(4) -0.076(7)
C41 0.126(10) 0.117(9) 0.038(5) -0.016(5) 0.022(6) -0.110(9)
C42 0.142(10) 0.064(6) 0.031(4) -0.002(4) 0.007(5) -0.078(7)
C43 0.086(6) 0.054(5) 0.035(4) 0.000(4) 0.002(4) -0.050(5)
C44 0.044(4) 0.028(3) 0.022(3) -0.001(2) -0.003(3) -0.017(3)
C45 0.037(4) 0.022(3) 0.024(3) 0.001(2) 0.001(3) -0.010(3)
C46 0.048(5) 0.035(4) 0.028(3) 0.002(3) 0.000(3) -0.018(3)
C47 0.066(6) 0.025(4) 0.039(4) 0.003(3) -0.003(4) -0.012(4)
C48 0.082(6) 0.025(4) 0.046(4) 0.001(3) -0.010(4) -0.028(4)
C49 0.053(5) 0.037(4) 0.034(4) 0.001(3) -0.003(3) -0.028(4)
C50 0.023(4) 0.054(5) 0.024(3) -0.002(3) 0.004(3) -0.022(3)
C51 0.025(4) 0.051(5) 0.038(4) 0.004(3) -0.003(3) -0.018(3)
C52 0.042(5) 0.057(5) 0.053(5) 0.002(4) -0.016(4) -0.012(4)
C53 0.040(5) 0.108(8) 0.047(5) 0.009(5) -0.021(4) -0.032(5)
C54 0.053(5) 0.082(7) 0.041(4) -0.013(4) -0.012(4) -0.035(5)
C55 0.037(4) 0.060(5) 0.037(4) -0.007(3) -0.003(3) -0.029(4)
C56 0.087(7) 0.048(5) 0.033(4) -0.013(3) -0.002(4) -0.030(5)
C57 0.043(5) 0.058(5) 0.054(5) 0.006(4) -0.018(4) -0.006(4)
C60 0.036(5) 0.100(7) 0.070(6) -0.008(5) -0.004(4) -0.038(5)
C61 0.045(5) 0.043(4) 0.045(4) -0.006(3) 0.006(3) -0.013(4)
C62 0.049(5) 0.056(5) 0.060(5) 0.005(4) 0.019(4) -0.004(4)
C63 0.046(5) 0.061(5) 0.052(5) 0.002(4) 0.006(4) -0.027(4)
C64 0.042(4) 0.034(4) 0.040(4) 0.013(3) 0.006(3) -0.012(3)

_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
C28A C27 1.582(10) . ?
C28A C29A 1.583(10) . ?
C29A C30 1.582(10) . ?
C28B C27 1.582(10) . ?
C28B C29B 1.583(10) . ?
C29B C30 1.583(10) . ?
C58A C57 1.510(7) . ?
C58A C59A 1.510(7) . ?
C59A C60 1.510(7) . ?
C58B C59B 1.510(7) . ?
C58B C57 1.510(7) . ?
C59B C60 1.510(7) . ?
Y1 C31 2.396(6) . ?
Y1 O3 2.408(5) . ?
Y1 O1 2.431(4) . ?
Y1 C51 2.480(7) . ?
Y1 C1 2.538(6) . ?
Y1 C15 2.567(7) . ?
Y1 C2 3.016(6) . ?
Y1 P1 3.319(2) . ?
Y1 Y2 3.6294(18) . ?
Y2 O4 2.450(5) . ?
Y2 C1 2.456(6) . ?
Y2 O5 2.471(4) . ?
Y2 C21 2.522(6) . ?
Y2 C45 2.572(6) . ?
Y2 C31 2.576(6) . ?
Y2 O2 2.577(4) . ?
P1 C1 1.701(6) . ?
P1 C20 1.807(7) . ?
P1 C14 1.811(7) . ?
P1 C8 1.851(6) . ?
P2 C31 1.714(6) . ?
P2 C50 1.819(7) . ?
P2 C44 1.824(7) . ?
P2 C38 1.830(6) . ?
O1 C33 1.404(8) . ?
O1 C56 1.446(8) . ?
O2 C3 1.398(7) . ?
O2 C26 1.445(7) . ?
O3 C30 1.434(9) . ?
O3 C27 1.450(10) . ?
O4 C60 1.447(9) . ?
O4 C57 1.447(9) . ?
O5 C64 1.447(6) . ?
O5 C61 1.453(8) . ?
C1 C2 1.449(9) . ?
C2 C7 1.413(9) . ?
C2 C3 1.437(9) . ?
C3 C4 1.350(9) . ?
C4 C5 1.402(10) . ?
C5 C6 1.379(12) . ?
C6 C7 1.381(10) . ?
C8 C9 1.381(11) . ?
C8 C13 1.395(10) . ?
C9 C10 1.379(11) . ?
C10 C11 1.362(14) . ?
C11 C12 1.349(14) . ?
C12 C13 1.402(11) . ?
C14 C19 1.407(9) . ?
C14 C15 1.407(9) . ?
C15 C16 1.414(9) . ?
C16 C17 1.368(10) . ?
C17 C18 1.379(12) . ?
C18 C19 1.387(11) . ?
C20 C25 1.391(9) . ?
C20 C21 1.423(9) . ?
C21 C22 1.383(10) . ?
C22 C23 1.381(10) . ?
C23 C24 1.392(12) . ?
C24 C25 1.376(11) . ?
C31 C32 1.455(8) . ?
C32 C37 1.408(9) . ?
C32 C33 1.418(9) . ?
C33 C34 1.359(9) . ?
C34 C35 1.382(11) . ?
C35 C36 1.368(11) . ?
C36 C37 1.410(10) . ?
C38 C43 1.380(11) . ?
C38 C39 1.411(11) . ?
C39 C40 1.387(10) . ?
C40 C41 1.371(15) . ?
C41 C42 1.380(15) . ?
C42 C43 1.398(10) . ?
C44 C49 1.404(9) . ?
C44 C45 1.405(9) . ?
C45 C46 1.427(9) . ?
C46 C47 1.378(10) . ?
C47 C48 1.373(11) . ?
C48 C49 1.380(10) . ?
C50 C51 1.395(10) . ?
C50 C55 1.406(9) . ?
C51 C52 1.388(10) . ?
C52 C53 1.409(12) . ?
C53 C54 1.361(12) . ?
C54 C55 1.377(11) . ?
C61 C62 1.522(10) . ?
C62 C63 1.498(11) . ?
C63 C64 1.512(8) . ?
O6 C68 1.4200 . ?
O6 C65 1.4200 . ?
C65 C66 1.4200 . ?
C66 C67 1.4200 . ?
C67 C68 1.4200 . ?
O7 C69 1.4200 . ?
O7 C72 1.4200 . ?
C69 C70 1.4200 . ?
C70 C71 1.4200 . ?
C71 C72 1.4200 . ?

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
C27 C28A C29A 95.4(14) . . ?
C30 C29A C28A 97.2(14) . . ?
C27 C28B C29B 93.4(13) . . ?
C30 C29B C28B 93.3(12) . . ?
C57 C58A C59A 93.9(9) . . ?
C58A C59A C60 115.6(10) . . ?
C59B C58B C57 118.5(11) . . ?
C60 C59B C58B 88.3(11) . . ?
C31 Y1 O3 109.18(19) . . ?
C31 Y1 O1 67.62(18) . . ?
O3 Y1 O1 76.41(17) . . ?
C31 Y1 C51 79.6(2) . . ?
O3 Y1 C51 87.5(2) . . ?
O1 Y1 C51 135.50(19) . . ?
C31 Y1 C1 87.5(2) . . ?
O3 Y1 C1 162.91(18) . . ?
O1 Y1 C1 108.11(18) . . ?
C51 Y1 C1 99.4(2) . . ?
C31 Y1 C15 146.1(2) . . ?
O3 Y1 C15 85.9(2) . . ?
O1 Y1 C15 87.93(19) . . ?
C51 Y1 C15 132.6(2) . . ?
C1 Y1 C15 77.9(2) . . ?
C31 Y1 C2 101.27(18) . . ?
O3 Y1 C2 142.82(18) . . ?
O1 Y1 C2 136.62(16) . . ?
C51 Y1 C2 77.35(19) . . ?
C1 Y1 C2 28.63(19) . . ?
C15 Y1 C2 80.17(19) . . ?
C31 Y1 P1 102.00(14) . . ?
O3 Y1 P1 136.87(14) . . ?
O1 Y1 P1 89.21(11) . . ?
C51 Y1 P1 127.69(15) . . ?
C1 Y1 P1 30.17(13) . . ?
C15 Y1 P1 52.63(16) . . ?
C2 Y1 P1 50.77(13) . . ?
C31 Y1 Y2 45.09(14) . . ?
O3 Y1 Y2 153.83(13) . . ?
O1 Y1 Y2 86.55(11) . . ?
C51 Y1 Y2 91.12(17) . . ?
C1 Y1 Y2 42.49(14) . . ?
C15 Y1 Y2 113.49(16) . . ?
C2 Y1 Y2 61.41(13) . . ?
P1 Y1 Y2 61.06(4) . . ?
O4 Y2 C1 139.06(18) . . ?
O4 Y2 O5 71.21(16) . . ?
C1 Y2 O5 91.43(17) . . ?
O4 Y2 C21 76.8(2) . . ?
C1 Y2 C21 75.1(2) . . ?
O5 Y2 C21 110.22(17) . . ?
O4 Y2 C45 82.34(19) . . ?
C1 Y2 C45 137.3(2) . . ?
O5 Y2 C45 95.02(17) . . ?
C21 Y2 C45 139.4(2) . . ?
O4 Y2 C31 121.93(18) . . ?
C1 Y2 C31 85.43(19) . . ?
O5 Y2 C31 161.48(18) . . ?
C21 Y2 C31 86.6(2) . . ?
C45 Y2 C31 75.45(19) . . ?
O4 Y2 O2 133.97(15) . . ?
C1 Y2 O2 64.75(17) . . ?
O5 Y2 O2 69.48(14) . . ?
C21 Y2 O2 139.72(18) . . ?
C45 Y2 O2 78.21(17) . . ?
C31 Y2 O2 92.79(17) . . ?
O4 Y2 Y1 148.99(12) . . ?
C1 Y2 Y1 44.27(13) . . ?
O5 Y2 Y1 133.48(11) . . ?
C21 Y2 Y1 76.33(16) . . ?
C45 Y2 Y1 108.96(15) . . ?
C31 Y2 Y1 41.20(14) . . ?
O2 Y2 Y1 77.04(10) . . ?
C1 P1 C20 107.8(3) . . ?
C1 P1 C14 115.4(3) . . ?
C20 P1 C14 106.0(3) . . ?
C1 P1 C8 115.3(3) . . ?
C20 P1 C8 104.6(3) . . ?
C14 P1 C8 107.0(3) . . ?
C1 P1 Y1 48.6(2) . . ?
C20 P1 Y1 90.9(2) . . ?
C14 P1 Y1 77.9(2) . . ?
C8 P1 Y1 161.4(2) . . ?
C31 P2 C50 109.2(3) . . ?
C31 P2 C44 114.4(3) . . ?
C50 P2 C44 108.8(3) . . ?
C31 P2 C38 113.8(3) . . ?
C50 P2 C38 104.4(3) . . ?
C44 P2 C38 105.8(3) . . ?
C33 O1 C56 115.6(5) . . ?
C33 O1 Y1 121.6(4) . . ?
C56 O1 Y1 122.3(4) . . ?
C3 O2 C26 115.2(5) . . ?
C3 O2 Y2 121.8(3) . . ?
C26 O2 Y2 123.0(4) . . ?
C30 O3 C27 110.5(6) . . ?
C30 O3 Y1 126.7(5) . . ?
C27 O3 Y1 118.5(5) . . ?
C60 O4 C57 109.0(6) . . ?
C60 O4 Y2 122.7(5) . . ?
C57 O4 Y2 125.8(4) . . ?
C64 O5 C61 106.0(4) . . ?
C64 O5 Y2 123.1(3) . . ?
C61 O5 Y2 128.8(4) . . ?
C2 C1 P1 119.9(4) . . ?
C2 C1 Y2 121.0(4) . . ?
P1 C1 Y2 115.6(3) . . ?
C2 C1 Y1 94.3(4) . . ?
P1 C1 Y1 101.3(3) . . ?
Y2 C1 Y1 93.24(19) . . ?
C7 C2 C3 112.9(6) . . ?
C7 C2 C1 127.8(6) . . ?
C3 C2 C1 119.3(5) . . ?
C7 C2 Y1 103.4(4) . . ?
C3 C2 Y1 109.8(4) . . ?
C1 C2 Y1 57.0(3) . . ?
C4 C3 O2 123.1(6) . . ?
C4 C3 C2 123.7(6) . . ?
O2 C3 C2 113.2(5) . . ?
C3 C4 C5 120.9(7) . . ?
C6 C5 C4 118.0(7) . . ?
C5 C6 C7 120.7(7) . . ?
C6 C7 C2 123.7(7) . . ?
C9 C8 C13 119.4(6) . . ?
C9 C8 P1 121.4(5) . . ?
C13 C8 P1 118.9(6) . . ?
C10 C9 C8 120.9(8) . . ?
C11 C10 C9 119.6(9) . . ?
C12 C11 C10 120.6(8) . . ?
C11 C12 C13 121.5(8) . . ?
C8 C13 C12 118.0(8) . . ?
C19 C14 C15 123.5(7) . . ?
C19 C14 P1 123.3(5) . . ?
C15 C14 P1 113.2(5) . . ?
C14 C15 C16 114.0(6) . . ?
C14 C15 Y1 116.3(5) . . ?
C16 C15 Y1 129.7(5) . . ?
C17 C16 C15 123.3(7) . . ?
C16 C17 C18 120.9(7) . . ?
C17 C18 C19 119.3(7) . . ?
C18 C19 C14 118.9(7) . . ?
C25 C20 C21 123.2(7) . . ?
C25 C20 P1 119.4(6) . . ?
C21 C20 P1 117.4(5) . . ?
C22 C21 C20 113.6(6) . . ?
C22 C21 Y2 127.0(5) . . ?
C20 C21 Y2 119.3(5) . . ?
C23 C22 C21 124.9(8) . . ?
C22 C23 C24 119.1(7) . . ?
C25 C24 C23 119.5(7) . . ?
C24 C25 C20 119.6(7) . . ?
O3 C27 C28A 100.6(11) . . ?
O3 C27 C28B 100.0(10) . . ?
C28A C27 C28B 50.7(11) . . ?
O3 C30 C29A 104.3(11) . . ?
O3 C30 C29B 101.3(11) . . ?
C29A C30 C29B 22.0(13) . . ?
C32 C31 P2 117.8(4) . . ?
C32 C31 Y1 118.1(4) . . ?
P2 C31 Y1 113.5(3) . . ?
C32 C31 Y2 103.3(4) . . ?
P2 C31 Y2 105.6(3) . . ?
Y1 C31 Y2 93.70(18) . . ?
C37 C32 C33 115.0(6) . . ?
C37 C32 C31 125.9(6) . . ?
C33 C32 C31 119.0(6) . . ?
C34 C33 O1 123.2(6) . . ?
C34 C33 C32 123.1(7) . . ?
O1 C33 C32 113.6(5) . . ?
C33 C34 C35 120.6(7) . . ?
C36 C35 C34 119.4(7) . . ?
C35 C36 C37 120.3(7) . . ?
C32 C37 C36 121.5(7) . . ?
C43 C38 C39 118.9(7) . . ?
C43 C38 P2 122.7(6) . . ?
C39 C38 P2 118.2(6) . . ?
C40 C39 C38 120.3(9) . . ?
C41 C40 C39 120.3(10) . . ?
C40 C41 C42 119.8(8) . . ?
C41 C42 C43 120.8(9) . . ?
C38 C43 C42 119.8(9) . . ?
C49 C44 C45 123.9(6) . . ?
C49 C44 P2 122.1(5) . . ?
C45 C44 P2 113.9(4) . . ?
C44 C45 C46 113.1(6) . . ?
C44 C45 Y2 119.1(4) . . ?
C46 C45 Y2 127.1(5) . . ?
C47 C46 C45 123.4(7) . . ?
C48 C47 C46 121.0(7) . . ?
C47 C48 C49 119.0(7) . . ?
C48 C49 C44 119.6(7) . . ?
C51 C50 C55 122.4(7) . . ?
C51 C50 P2 119.2(5) . . ?
C55 C50 P2 118.3(6) . . ?
C52 C51 C50 115.6(7) . . ?
C52 C51 Y1 127.7(5) . . ?
C50 C51 Y1 116.0(5) . . ?
C51 C52 C53 122.8(8) . . ?
C54 C53 C52 119.4(8) . . ?
C53 C54 C55 120.3(7) . . ?
C54 C55 C50 119.5(8) . . ?
O4 C57 C58A 114.7(7) . . ?
O4 C57 C58B 96.9(9) . . ?
C58A C57 C58B 19.4(8) . . ?
O4 C60 C59B 114.0(9) . . ?
O4 C60 C59A 98.3(8) . . ?
C59B C60 C59A 46.4(9) . . ?
O5 C61 C62 105.3(6) . . ?
C63 C62 C61 105.4(6) . . ?
C62 C63 C64 104.9(6) . . ?
O5 C64 C63 103.2(5) . . ?
C68 O6 C65 108.0 . . ?
O6 C65 C66 108.0 . . ?
C67 C66 C65 108.0 . . ?
C66 C67 C68 108.0 . . ?
O6 C68 C67 108.0 . . ?
C69 O7 C72 108.0 . . ?
C70 C69 O7 108.0 . . ?
C69 C70 C71 108.0 . . ?
C72 C71 C70 108.0 . . ?
C71 C72 O7 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.101