data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'P G Edwards'
_publ_contact_author_email       EDWARDSPG@CARDIFF.AC.UK

_publ_section_title              
;
Coordination chemistry of cis,cis and trans,trans
1,1'-[1,2-phenylenebis(methylene)]bis(2,2,3,4,4-pentamethylphosphetane)
;
loop_
_publ_author_name
'P G Edwards'
'Dennis Coleman'
'Graham R Eastham'
'Benson M Kariuki'
'Paul David Newman'

# Attachment 'Compound_5.CIF'

data_compound5
_database_code_depnum_ccdc_archive 'CCDC 756177'
#TrackingRef 'Compound_5.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H40 P2'
_chemical_formula_sum            'C24 H40 P2'
_chemical_formula_weight         390.50

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'

_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                   6.0343(3)
_cell_length_b                   13.2316(8)
_cell_length_c                   15.4746(10)
_cell_angle_alpha                83.084(3)
_cell_angle_beta                 79.072(3)
_cell_angle_gamma                87.465(3)
_cell_volume                     1204.02(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3029
_cell_measurement_theta_min      3.92
_cell_measurement_theta_max      25.32

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             428
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9726
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_process_details   Denzo/Scalepack

_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  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13420
_diffrn_reflns_av_R_equivalents  0.1640
_diffrn_reflns_av_sigmaI/netI    0.1374
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.92
_diffrn_reflns_theta_max         25.32
_reflns_number_total             4369
_reflns_number_gt                3029
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    SHELXs-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ?
_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^)+(0.1059P)^2^+1.5883P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4369
_refine_ls_number_parameters     245
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0900
_refine_ls_wR_factor_ref         0.2368
_refine_ls_wR_factor_gt          0.2117
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.065
_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
P1 P 0.71947(19) 0.14837(8) 0.21184(7) 0.0244(3) Uani 1 1 d . . .
P2 P 0.5569(2) 0.46902(8) 0.29381(9) 0.0310(4) Uani 1 1 d . . .
C1 C 0.5822(8) 0.2156(3) 0.3773(3) 0.0297(10) Uani 1 1 d . . .
C2 C 0.3884(8) 0.2781(3) 0.3721(3) 0.0271(10) Uani 1 1 d . . .
C3 C 0.2033(9) 0.2645(4) 0.4430(3) 0.0382(12) Uani 1 1 d . . .
H3 H 0.0715 0.3062 0.4413 0.046 Uiso 1 1 calc R . .
C4 C 0.2086(10) 0.1927(4) 0.5143(4) 0.0459(14) Uani 1 1 d . . .
H4 H 0.0806 0.1847 0.5607 0.055 Uiso 1 1 calc R . .
C5 C 0.3978(12) 0.1323(4) 0.5190(4) 0.0515(16) Uani 1 1 d . . .
H5 H 0.4020 0.0828 0.5685 0.062 Uiso 1 1 calc R . .
C6 C 0.5828(10) 0.1447(3) 0.4503(3) 0.0389(12) Uani 1 1 d . . .
H6 H 0.7139 0.1030 0.4537 0.047 Uiso 1 1 calc R . .
C7 C 0.7796(8) 0.2201(3) 0.3011(3) 0.0302(10) Uani 1 1 d . . .
H7A H 0.9159 0.1905 0.3222 0.036 Uiso 1 1 calc R . .
H7B H 0.8098 0.2920 0.2771 0.036 Uiso 1 1 calc R . .
C8 C 0.9402(7) 0.1842(3) 0.1105(3) 0.0276(10) Uani 1 1 d . . .
C9 C 1.0089(7) 0.0689(3) 0.1096(3) 0.0280(10) Uani 1 1 d . . .
H9 H 0.9163 0.0401 0.0716 0.034 Uiso 1 1 calc R . .
C10 C 0.9059(8) 0.0301(3) 0.2078(3) 0.0275(10) Uani 1 1 d . . .
C11 C 0.8454(9) 0.2294(4) 0.0295(3) 0.0424(12) Uani 1 1 d . . .
H11A H 0.7907 0.2992 0.0370 0.064 Uiso 1 1 calc R . .
H11B H 0.7203 0.1881 0.0226 0.064 Uiso 1 1 calc R . .
H11C H 0.9643 0.2300 -0.0234 0.064 Uiso 1 1 calc R . .
C12 C 1.1278(8) 0.2516(4) 0.1235(3) 0.0363(11) Uani 1 1 d . . .
H12A H 1.2431 0.2591 0.0694 0.055 Uiso 1 1 calc R . .
H12B H 1.1963 0.2202 0.1730 0.055 Uiso 1 1 calc R . .
H12C H 1.0643 0.3188 0.1364 0.055 Uiso 1 1 calc R . .
C13 C 1.2538(8) 0.0419(4) 0.0742(4) 0.0411(12) Uani 1 1 d . . .
H13A H 1.3503 0.0667 0.1111 0.062 Uiso 1 1 calc R . .
H13B H 1.2969 0.0737 0.0131 0.062 Uiso 1 1 calc R . .
H13C H 1.2723 -0.0322 0.0756 0.062 Uiso 1 1 calc R . .
C14 C 1.0772(8) 0.0159(4) 0.2707(3) 0.0350(11) Uani 1 1 d . . .
H14A H 0.9962 0.0044 0.3321 0.053 Uiso 1 1 calc R . .
H14B H 1.1676 0.0772 0.2630 0.053 Uiso 1 1 calc R . .
H14C H 1.1767 -0.0429 0.2571 0.053 Uiso 1 1 calc R . .
C15 C 0.7757(9) -0.0687(3) 0.2154(4) 0.0384(12) Uani 1 1 d . . .
H15A H 0.8798 -0.1231 0.1940 0.058 Uiso 1 1 calc R . .
H15B H 0.6574 -0.0580 0.1795 0.058 Uiso 1 1 calc R . .
H15C H 0.7068 -0.0882 0.2775 0.058 Uiso 1 1 calc R . .
C16 C 0.3776(8) 0.3576(3) 0.2956(3) 0.0306(10) Uani 1 1 d . . .
H16A H 0.2190 0.3815 0.2981 0.037 Uiso 1 1 calc R . .
H16B H 0.4262 0.3264 0.2398 0.037 Uiso 1 1 calc R . .
C17 C 0.3661(9) 0.5754(4) 0.3401(4) 0.0408(13) Uani 1 1 d . . .
C18 C 0.4459(17) 0.6387(6) 0.2496(6) 0.091(3) Uani 1 1 d U . .
H18 H 0.5870 0.6725 0.2549 0.109 Uiso 1 1 calc R . .
C19 C 0.5208(10) 0.5547(4) 0.1905(4) 0.0450(13) Uani 1 1 d . . .
C20 C 0.4481(15) 0.6236(6) 0.4110(6) 0.095(3) Uani 1 1 d U . .
H20A H 0.3726 0.6901 0.4175 0.143 Uiso 1 1 calc R . .
H20B H 0.6117 0.6325 0.3945 0.143 Uiso 1 1 calc R . .
H20C H 0.4135 0.5796 0.4673 0.143 Uiso 1 1 calc R . .
C21 C 0.1204(13) 0.5544(6) 0.3686(7) 0.100(3) Uani 1 1 d U . .
H21A H 0.0970 0.5075 0.4234 0.149 Uiso 1 1 calc R . .
H21B H 0.0663 0.5237 0.3221 0.149 Uiso 1 1 calc R . .
H21C H 0.0367 0.6183 0.3790 0.149 Uiso 1 1 calc R . .
C22 C 0.2867(14) 0.7244(5) 0.2207(6) 0.080(2) Uani 1 1 d U . .
H22A H 0.1425 0.6957 0.2168 0.120 Uiso 1 1 calc R . .
H22B H 0.3551 0.7586 0.1627 0.120 Uiso 1 1 calc R . .
H22C H 0.2607 0.7737 0.2642 0.120 Uiso 1 1 calc R . .
C23 C 0.7448(16) 0.5811(8) 0.1289(6) 0.108(3) Uani 1 1 d U . .
H23A H 0.7949 0.5250 0.0935 0.161 Uiso 1 1 calc R . .
H23B H 0.8584 0.5921 0.1643 0.161 Uiso 1 1 calc R . .
H23C H 0.7249 0.6433 0.0896 0.161 Uiso 1 1 calc R . .
C24 C 0.3713(14) 0.5196(5) 0.1331(5) 0.075(2) Uani 1 1 d . . .
H24A H 0.3458 0.5755 0.0882 0.113 Uiso 1 1 calc R . .
H24B H 0.2263 0.4986 0.1698 0.113 Uiso 1 1 calc R . .
H24C H 0.4441 0.4618 0.1039 0.113 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0240(6) 0.0220(6) 0.0293(6) -0.0108(4) -0.0055(5) 0.0008(4)
P2 0.0333(7) 0.0197(6) 0.0431(7) -0.0069(5) -0.0131(6) -0.0007(5)
C1 0.041(3) 0.018(2) 0.033(2) -0.0141(18) -0.010(2) 0.0013(19)
C2 0.032(2) 0.020(2) 0.032(2) -0.0124(18) -0.0050(19) -0.0012(18)
C3 0.041(3) 0.028(2) 0.045(3) -0.016(2) 0.002(2) -0.004(2)
C4 0.065(4) 0.029(3) 0.039(3) -0.014(2) 0.009(3) -0.007(3)
C5 0.095(5) 0.027(3) 0.031(3) -0.004(2) -0.006(3) -0.007(3)
C6 0.061(3) 0.023(2) 0.034(3) -0.009(2) -0.009(3) 0.005(2)
C7 0.035(3) 0.026(2) 0.033(2) -0.0119(19) -0.009(2) 0.0048(19)
C8 0.026(2) 0.028(2) 0.029(2) 0.0003(18) -0.0065(19) -0.0029(18)
C9 0.027(2) 0.030(2) 0.030(2) -0.0144(19) -0.0036(19) -0.0025(18)
C10 0.031(2) 0.020(2) 0.032(2) -0.0077(18) -0.0055(19) 0.0034(18)
C11 0.047(3) 0.046(3) 0.034(3) 0.003(2) -0.012(2) -0.004(2)
C12 0.033(3) 0.037(3) 0.040(3) -0.007(2) -0.004(2) -0.008(2)
C13 0.031(3) 0.050(3) 0.045(3) -0.022(2) -0.003(2) 0.002(2)
C14 0.039(3) 0.028(2) 0.041(3) -0.009(2) -0.013(2) 0.007(2)
C15 0.050(3) 0.021(2) 0.046(3) -0.009(2) -0.010(2) 0.001(2)
C16 0.032(2) 0.021(2) 0.042(3) -0.0125(19) -0.008(2) -0.0021(18)
C17 0.044(3) 0.024(2) 0.063(3) -0.018(2) -0.026(3) 0.009(2)
C18 0.128(6) 0.051(4) 0.098(5) -0.004(4) -0.041(5) 0.029(4)
C19 0.056(3) 0.028(3) 0.052(3) 0.003(2) -0.018(3) -0.007(2)
C20 0.100(5) 0.078(5) 0.133(6) -0.078(5) -0.056(5) 0.027(4)
C21 0.071(5) 0.066(4) 0.163(7) -0.065(5) 0.006(5) 0.007(4)
C22 0.100(5) 0.039(3) 0.111(5) -0.005(3) -0.048(5) 0.014(3)
C23 0.093(6) 0.129(7) 0.094(6) 0.045(5) -0.027(5) -0.045(5)
C24 0.108(6) 0.049(4) 0.083(5) 0.015(3) -0.063(5) -0.020(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
P1 C7 1.864(4) . ?
P1 C8 1.882(5) . ?
P1 C10 1.887(4) . ?
P2 C16 1.862(4) . ?
P2 C19 1.888(5) . ?
P2 C17 1.899(5) . ?
C1 C6 1.380(7) . ?
C1 C2 1.412(6) . ?
C1 C7 1.507(7) . ?
C2 C3 1.411(7) . ?
C2 C16 1.494(6) . ?
C3 C4 1.370(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C11 1.523(6) . ?
C8 C12 1.528(6) . ?
C8 C9 1.565(6) . ?
C9 C13 1.518(6) . ?
C9 C10 1.562(6) . ?
C9 H9 1.0000 . ?
C10 C15 1.536(6) . ?
C10 C14 1.540(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C21 1.493(10) . ?
C17 C20 1.503(8) . ?
C17 C18 1.546(10) . ?
C18 C19 1.525(10) . ?
C18 C22 1.534(9) . ?
C18 H18 1.0000 . ?
C19 C24 1.502(8) . ?
C19 C23 1.526(10) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 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
C7 P1 C8 107.0(2) . . ?
C7 P1 C10 108.56(19) . . ?
C8 P1 C10 78.18(19) . . ?
C16 P2 C19 104.9(2) . . ?
C16 P2 C17 107.8(2) . . ?
C19 P2 C17 77.5(2) . . ?
C6 C1 C2 119.3(5) . . ?
C6 C1 C7 119.9(4) . . ?
C2 C1 C7 120.6(4) . . ?
C3 C2 C1 117.6(4) . . ?
C3 C2 C16 120.4(4) . . ?
C1 C2 C16 122.0(4) . . ?
C4 C3 C2 121.7(5) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 120.4(5) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 119.0(5) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C1 C6 C5 122.0(5) . . ?
C1 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C1 C7 P1 110.5(3) . . ?
C1 C7 H7A 109.6 . . ?
P1 C7 H7A 109.6 . . ?
C1 C7 H7B 109.6 . . ?
P1 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C11 C8 C12 109.3(4) . . ?
C11 C8 C9 113.5(4) . . ?
C12 C8 C9 114.2(4) . . ?
C11 C8 P1 114.3(3) . . ?
C12 C8 P1 115.8(3) . . ?
C9 C8 P1 88.6(3) . . ?
C13 C9 C10 118.5(4) . . ?
C13 C9 C8 118.0(4) . . ?
C10 C9 C8 99.0(3) . . ?
C13 C9 H9 106.8 . . ?
C10 C9 H9 106.8 . . ?
C8 C9 H9 106.8 . . ?
C15 C10 C14 109.3(4) . . ?
C15 C10 C9 112.2(4) . . ?
C14 C10 C9 114.7(4) . . ?
C15 C10 P1 113.7(3) . . ?
C14 C10 P1 117.2(3) . . ?
C9 C10 P1 88.5(3) . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C2 C16 P2 113.3(3) . . ?
C2 C16 H16A 108.9 . . ?
P2 C16 H16A 108.9 . . ?
C2 C16 H16B 108.9 . . ?
P2 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C21 C17 C20 109.4(6) . . ?
C21 C17 C18 118.5(6) . . ?
C20 C17 C18 109.1(6) . . ?
C21 C17 P2 117.4(4) . . ?
C20 C17 P2 114.5(4) . . ?
C18 C17 P2 86.4(4) . . ?
C19 C18 C22 119.5(7) . . ?
C19 C18 C17 101.1(5) . . ?
C22 C18 C17 117.1(8) . . ?
C19 C18 H18 106.0 . . ?
C22 C18 H18 106.0 . . ?
C17 C18 H18 106.0 . . ?
C24 C19 C18 121.8(6) . . ?
C24 C19 C23 105.9(6) . . ?
C18 C19 C23 110.3(7) . . ?
C24 C19 P2 117.9(4) . . ?
C18 C19 P2 87.4(4) . . ?
C23 C19 P2 112.9(5) . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.32
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.293
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.083

# Attachment 'Compound_10.CIF'

data_compound10
_database_code_depnum_ccdc_archive 'CCDC 756178'
#TrackingRef 'Compound_10.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H40 Mo O4 P2'
_chemical_formula_sum            'C28 H40 Mo O4 P2'
_chemical_formula_weight         598.48

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.5960(2)
_cell_length_b                   17.2901(3)
_cell_length_c                   13.8362(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.5887(7)
_cell_angle_gamma                90.00
_cell_volume                     2902.49(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5663
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      27.49

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8907
_exptl_absorpt_correction_T_max  0.9653
_exptl_absorpt_process_details   Denzo/Scalepack

_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  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39770
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6638
_reflns_number_gt                5663
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    SHELXs-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ?
_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^)+(0.0261P)^2^+2.5476P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6638
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0748
_refine_ls_wR_factor_gt          0.0707
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
Mo1 Mo 0.539297(14) 0.142951(10) 0.304569(13) 0.01610(6) Uani 1 1 d . . .
P1 P 0.38038(4) 0.22470(3) 0.20309(4) 0.01740(11) Uani 1 1 d . . .
P2 P 0.64415(4) 0.11765(3) 0.17406(4) 0.01704(11) Uani 1 1 d . . .
O1 O 0.43802(15) 0.14925(11) 0.48889(13) 0.0392(4) Uani 1 1 d . . .
O2 O 0.39783(15) -0.00541(11) 0.21501(17) 0.0496(5) Uani 1 1 d . . .
O3 O 0.71394(14) 0.04437(10) 0.46093(12) 0.0346(4) Uani 1 1 d . . .
O4 O 0.67355(13) 0.30049(10) 0.35350(13) 0.0322(4) Uani 1 1 d . . .
C1 C 0.47176(18) 0.14953(13) 0.41906(17) 0.0246(5) Uani 1 1 d . . .
C2 C 0.44914(18) 0.04773(14) 0.24980(18) 0.0279(5) Uani 1 1 d . . .
C3 C 0.65242(18) 0.08009(13) 0.40032(16) 0.0231(5) Uani 1 1 d . . .
C4 C 0.62565(17) 0.24357(13) 0.33824(16) 0.0215(4) Uani 1 1 d . . .
C5 C 0.38365(16) 0.25006(13) 0.07361(15) 0.0203(4) Uani 1 1 d . . .
H5A H 0.3718 0.2022 0.0329 0.024 Uiso 1 1 calc R . .
H5B H 0.3209 0.2850 0.0446 0.024 Uiso 1 1 calc R . .
C6 C 0.48815(16) 0.28842(12) 0.06319(14) 0.0182(4) Uani 1 1 d . . .
C7 C 0.49194(18) 0.36912(13) 0.06066(16) 0.0224(5) Uani 1 1 d . . .
H7 H 0.4315 0.3978 0.0707 0.027 Uiso 1 1 calc R . .
C8 C 0.58107(18) 0.40877(13) 0.04398(16) 0.0252(5) Uani 1 1 d . . .
H8 H 0.5826 0.4637 0.0453 0.030 Uiso 1 1 calc R . .
C9 C 0.66786(19) 0.36773(13) 0.02540(18) 0.0272(5) Uani 1 1 d . . .
H9 H 0.7286 0.3940 0.0121 0.033 Uiso 1 1 calc R . .
C10 C 0.66465(18) 0.28810(13) 0.02650(16) 0.0237(5) Uani 1 1 d . . .
H10 H 0.7238 0.2600 0.0128 0.028 Uiso 1 1 calc R . .
C11 C 0.57766(17) 0.24713(12) 0.04710(14) 0.0184(4) Uani 1 1 d . . .
C12 C 0.58394(18) 0.15955(12) 0.04766(15) 0.0211(4) Uani 1 1 d . . .
H12A H 0.6289 0.1430 0.0026 0.025 Uiso 1 1 calc R . .
H12B H 0.5088 0.1385 0.0203 0.025 Uiso 1 1 calc R . .
C13 C 0.23272(16) 0.19501(13) 0.19569(16) 0.0227(5) Uani 1 1 d . . .
C14 C 0.23331(18) 0.25841(14) 0.27630(18) 0.0282(5) Uani 1 1 d . . .
H14 H 0.2599 0.2331 0.3435 0.034 Uiso 1 1 calc R . .
C15 C 0.32800(17) 0.31132(13) 0.26273(17) 0.0236(5) Uani 1 1 d . . .
C16 C 0.21260(19) 0.11483(15) 0.2322(2) 0.0338(6) Uani 1 1 d . . .
H16A H 0.1407 0.1137 0.2469 0.051 Uiso 1 1 calc R . .
H16B H 0.2706 0.1024 0.2932 0.051 Uiso 1 1 calc R . .
H16C H 0.2135 0.0767 0.1800 0.051 Uiso 1 1 calc R . .
C17 C 0.15207(19) 0.20867(17) 0.09326(18) 0.0359(6) Uani 1 1 d . . .
H17A H 0.1654 0.1707 0.0453 0.054 Uiso 1 1 calc R . .
H17B H 0.1625 0.2610 0.0700 0.054 Uiso 1 1 calc R . .
H17C H 0.0764 0.2031 0.0986 0.054 Uiso 1 1 calc R . .
C18 C 0.1224(2) 0.29665(16) 0.2726(2) 0.0360(6) Uani 1 1 d . . .
H18A H 0.1331 0.3363 0.3249 0.054 Uiso 1 1 calc R . .
H18B H 0.0708 0.2574 0.2838 0.054 Uiso 1 1 calc R . .
H18C H 0.0924 0.3206 0.2067 0.054 Uiso 1 1 calc R . .
C19 C 0.2906(2) 0.38164(14) 0.1959(2) 0.0353(6) Uani 1 1 d . . .
H19A H 0.2466 0.4156 0.2267 0.053 Uiso 1 1 calc R . .
H19B H 0.2459 0.3647 0.1299 0.053 Uiso 1 1 calc R . .
H19C H 0.3553 0.4098 0.1881 0.053 Uiso 1 1 calc R . .
C20 C 0.4033(2) 0.34033(15) 0.36239(19) 0.0343(6) Uani 1 1 d . . .
H20A H 0.4659 0.3682 0.3497 0.051 Uiso 1 1 calc R . .
H20B H 0.4303 0.2962 0.4065 0.051 Uiso 1 1 calc R . .
H20C H 0.3617 0.3751 0.3946 0.051 Uiso 1 1 calc R . .
C21 C 0.80091(17) 0.12653(13) 0.21102(16) 0.0220(5) Uani 1 1 d . . .
C22 C 0.80495(17) 0.03684(13) 0.22501(18) 0.0255(5) Uani 1 1 d . . .
H22 H 0.8030 0.0266 0.2957 0.031 Uiso 1 1 calc R . .
C23 C 0.68894(17) 0.01469(13) 0.15616(17) 0.0235(5) Uani 1 1 d . . .
C24 C 0.85329(19) 0.17036(15) 0.30796(18) 0.0302(5) Uani 1 1 d . . .
H24A H 0.9322 0.1584 0.3302 0.045 Uiso 1 1 calc R . .
H24B H 0.8180 0.1547 0.3599 0.045 Uiso 1 1 calc R . .
H24C H 0.8433 0.2261 0.2959 0.045 Uiso 1 1 calc R . .
C25 C 0.85475(18) 0.15470(15) 0.13068(19) 0.0298(5) Uani 1 1 d . . .
H25A H 0.8535 0.2114 0.1286 0.045 Uiso 1 1 calc R . .
H25B H 0.8140 0.1343 0.0652 0.045 Uiso 1 1 calc R . .
H25C H 0.9312 0.1366 0.1468 0.045 Uiso 1 1 calc R . .
C26 C 0.9048(2) -0.00600(15) 0.2096(2) 0.0354(6) Uani 1 1 d . . .
H26A H 0.8989 -0.0611 0.2239 0.053 Uiso 1 1 calc R . .
H26B H 0.9721 0.0152 0.2549 0.053 Uiso 1 1 calc R . .
H26C H 0.9077 0.0004 0.1400 0.053 Uiso 1 1 calc R . .
C27 C 0.6868(2) -0.00567(14) 0.04773(18) 0.0315(5) Uani 1 1 d . . .
H27A H 0.7219 -0.0561 0.0464 0.047 Uiso 1 1 calc R . .
H27B H 0.7269 0.0339 0.0210 0.047 Uiso 1 1 calc R . .
H27C H 0.6102 -0.0078 0.0066 0.047 Uiso 1 1 calc R . .
C28 C 0.6370(2) -0.05238(13) 0.19886(19) 0.0309(5) Uani 1 1 d . . .
H28A H 0.5632 -0.0627 0.1551 0.046 Uiso 1 1 calc R . .
H28B H 0.6316 -0.0389 0.2662 0.046 Uiso 1 1 calc R . .
H28C H 0.6829 -0.0987 0.2027 0.046 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.01525(10) 0.01720(10) 0.01623(9) 0.00125(7) 0.00492(7) -0.00067(7)
P1 0.0146(2) 0.0199(3) 0.0181(3) 0.0015(2) 0.0052(2) -0.0008(2)
P2 0.0165(2) 0.0163(3) 0.0189(3) -0.0013(2) 0.0059(2) -0.0010(2)
O1 0.0395(10) 0.0554(12) 0.0295(9) 0.0018(8) 0.0212(8) -0.0027(9)
O2 0.0376(10) 0.0322(11) 0.0852(15) -0.0185(10) 0.0270(10) -0.0141(9)
O3 0.0377(10) 0.0341(10) 0.0281(9) 0.0055(8) 0.0024(8) 0.0100(8)
O4 0.0325(9) 0.0248(9) 0.0386(9) -0.0030(7) 0.0086(8) -0.0084(7)
C1 0.0200(11) 0.0285(12) 0.0244(11) 0.0018(9) 0.0043(9) -0.0008(9)
C2 0.0230(11) 0.0255(13) 0.0383(13) -0.0006(10) 0.0134(10) -0.0025(9)
C3 0.0247(11) 0.0241(12) 0.0208(10) -0.0024(9) 0.0065(9) 0.0002(9)
C4 0.0186(10) 0.0256(12) 0.0200(10) 0.0006(9) 0.0046(8) 0.0020(9)
C5 0.0173(10) 0.0257(12) 0.0181(10) 0.0031(8) 0.0051(8) 0.0006(8)
C6 0.0179(10) 0.0241(11) 0.0126(9) 0.0012(8) 0.0041(8) -0.0018(8)
C7 0.0218(11) 0.0241(12) 0.0225(11) 0.0017(9) 0.0080(9) 0.0028(9)
C8 0.0285(12) 0.0202(11) 0.0275(11) 0.0023(9) 0.0085(10) -0.0027(9)
C9 0.0232(11) 0.0284(13) 0.0318(12) 0.0031(10) 0.0104(10) -0.0062(9)
C10 0.0207(11) 0.0261(12) 0.0268(11) 0.0016(9) 0.0107(9) 0.0010(9)
C11 0.0222(10) 0.0197(11) 0.0133(9) 0.0008(8) 0.0051(8) -0.0012(8)
C12 0.0230(11) 0.0244(11) 0.0172(10) -0.0018(8) 0.0074(9) -0.0001(9)
C13 0.0151(10) 0.0281(12) 0.0257(11) 0.0024(9) 0.0068(9) -0.0005(9)
C14 0.0242(11) 0.0342(13) 0.0298(12) 0.0075(10) 0.0136(10) 0.0037(10)
C15 0.0233(11) 0.0241(12) 0.0263(11) 0.0010(9) 0.0118(9) 0.0027(9)
C16 0.0213(11) 0.0374(14) 0.0431(14) 0.0104(12) 0.0092(11) -0.0058(10)
C17 0.0189(11) 0.0565(18) 0.0317(13) 0.0060(12) 0.0058(10) -0.0041(11)
C18 0.0294(13) 0.0420(15) 0.0428(14) 0.0061(12) 0.0202(11) 0.0074(11)
C19 0.0449(15) 0.0264(13) 0.0430(15) 0.0076(11) 0.0260(13) 0.0109(11)
C20 0.0379(14) 0.0331(14) 0.0349(13) -0.0067(11) 0.0151(12) 0.0011(11)
C21 0.0161(10) 0.0248(12) 0.0255(11) -0.0009(9) 0.0065(9) -0.0004(8)
C22 0.0204(11) 0.0253(12) 0.0315(12) 0.0012(10) 0.0084(9) 0.0032(9)
C23 0.0228(11) 0.0190(11) 0.0303(12) -0.0041(9) 0.0097(9) 0.0019(9)
C24 0.0221(11) 0.0351(14) 0.0321(13) -0.0041(11) 0.0047(10) -0.0029(10)
C25 0.0201(11) 0.0353(14) 0.0363(13) 0.0053(11) 0.0117(10) -0.0015(10)
C26 0.0288(13) 0.0301(14) 0.0491(15) 0.0025(12) 0.0133(12) 0.0095(10)
C27 0.0381(13) 0.0247(12) 0.0343(13) -0.0073(10) 0.0143(11) 0.0009(10)
C28 0.0336(13) 0.0189(12) 0.0416(14) 0.0004(10) 0.0124(11) 0.0010(10)

_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
Mo1 C3 1.988(2) . ?
Mo1 C1 1.993(2) . ?
Mo1 C2 2.028(2) . ?
Mo1 C4 2.038(2) . ?
Mo1 P1 2.5427(5) . ?
Mo1 P2 2.5451(6) . ?
P1 C5 1.856(2) . ?
P1 C13 1.906(2) . ?
P1 C15 1.911(2) . ?
P2 C12 1.856(2) . ?
P2 C23 1.904(2) . ?
P2 C21 1.908(2) . ?
O1 C1 1.155(3) . ?
O2 C2 1.152(3) . ?
O3 C3 1.156(3) . ?
O4 C4 1.144(3) . ?
C5 C6 1.515(3) . ?
C6 C7 1.397(3) . ?
C6 C11 1.402(3) . ?
C7 C8 1.387(3) . ?
C8 C9 1.384(3) . ?
C9 C10 1.378(3) . ?
C10 C11 1.397(3) . ?
C11 C12 1.516(3) . ?
C13 C16 1.520(3) . ?
C13 C17 1.524(3) . ?
C13 C14 1.562(3) . ?
C14 C18 1.534(3) . ?
C14 C15 1.554(3) . ?
C15 C19 1.523(3) . ?
C15 C20 1.533(3) . ?
C21 C24 1.527(3) . ?
C21 C25 1.529(3) . ?
C21 C22 1.562(3) . ?
C22 C26 1.523(3) . ?
C22 C23 1.563(3) . ?
C23 C28 1.526(3) . ?
C23 C27 1.534(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
C3 Mo1 C1 83.35(9) . . ?
C3 Mo1 C2 91.96(9) . . ?
C1 Mo1 C2 91.58(9) . . ?
C3 Mo1 C4 94.10(9) . . ?
C1 Mo1 C4 94.89(9) . . ?
C2 Mo1 C4 171.60(9) . . ?
C3 Mo1 P1 171.42(6) . . ?
C1 Mo1 P1 88.07(6) . . ?
C2 Mo1 P1 88.07(7) . . ?
C4 Mo1 P1 86.81(6) . . ?
C3 Mo1 P2 87.89(6) . . ?
C1 Mo1 P2 170.98(7) . . ?
C2 Mo1 P2 86.59(7) . . ?
C4 Mo1 P2 87.82(6) . . ?
P1 Mo1 P2 100.682(18) . . ?
C5 P1 C13 106.64(9) . . ?
C5 P1 C15 109.36(10) . . ?
C13 P1 C15 77.82(10) . . ?
C5 P1 Mo1 116.50(7) . . ?
C13 P1 Mo1 119.48(7) . . ?
C15 P1 Mo1 120.60(7) . . ?
C12 P2 C23 107.61(10) . . ?
C12 P2 C21 110.64(10) . . ?
C23 P2 C21 77.80(9) . . ?
C12 P2 Mo1 116.29(7) . . ?
C23 P2 Mo1 118.78(7) . . ?
C21 P2 Mo1 119.53(7) . . ?
O1 C1 Mo1 175.0(2) . . ?
O2 C2 Mo1 177.4(2) . . ?
O3 C3 Mo1 175.11(19) . . ?
O4 C4 Mo1 177.53(19) . . ?
C6 C5 P1 116.14(14) . . ?
C7 C6 C11 118.05(19) . . ?
C7 C6 C5 118.43(18) . . ?
C11 C6 C5 123.28(19) . . ?
C8 C7 C6 122.2(2) . . ?
C9 C8 C7 119.5(2) . . ?
C10 C9 C8 118.9(2) . . ?
C9 C10 C11 122.4(2) . . ?
C10 C11 C6 118.86(19) . . ?
C10 C11 C12 117.69(19) . . ?
C6 C11 C12 123.42(18) . . ?
C11 C12 P2 113.71(14) . . ?
C16 C13 C17 108.75(19) . . ?
C16 C13 C14 111.83(19) . . ?
C17 C13 C14 115.4(2) . . ?
C16 C13 P1 118.38(15) . . ?
C17 C13 P1 113.92(15) . . ?
C14 C13 P1 87.44(13) . . ?
C18 C14 C15 117.6(2) . . ?
C18 C14 C13 116.7(2) . . ?
C15 C14 C13 100.57(17) . . ?
C19 C15 C20 107.5(2) . . ?
C19 C15 C14 114.90(19) . . ?
C20 C15 C14 113.15(19) . . ?
C19 C15 P1 116.72(16) . . ?
C20 C15 P1 116.30(16) . . ?
C14 C15 P1 87.48(14) . . ?
C24 C21 C25 108.00(19) . . ?
C24 C21 C22 113.07(19) . . ?
C25 C21 C22 113.60(19) . . ?
C24 C21 P2 116.55(15) . . ?
C25 C21 P2 117.39(15) . . ?
C22 C21 P2 87.15(13) . . ?
C26 C22 C21 117.77(19) . . ?
C26 C22 C23 117.9(2) . . ?
C21 C22 C23 100.01(17) . . ?
C28 C23 C27 107.90(19) . . ?
C28 C23 C22 112.21(19) . . ?
C27 C23 C22 114.86(18) . . ?
C28 C23 P2 119.17(15) . . ?
C27 C23 P2 114.45(16) . . ?
C22 C23 P2 87.29(13) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.116

# Attachment 'Compound_11.CIF'

data_compound11
_database_code_depnum_ccdc_archive 'CCDC 756179'
#TrackingRef 'Compound_11.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H42 Cl4 P2 Pd'
_chemical_formula_sum            'C25 H42 Cl4 P2 Pd'
_chemical_formula_weight         652.73

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   8.78660(10)
_cell_length_b                   10.8661(2)
_cell_length_c                   15.9424(3)
_cell_angle_alpha                109.6672(8)
_cell_angle_beta                 93.1967(8)
_cell_angle_gamma                95.8861(10)
_cell_volume                     1419.13(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5559
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      27.51

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7229
_exptl_absorpt_correction_T_max  0.7609
_exptl_absorpt_process_details   Denzo/Scalepack

_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  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26820
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         27.51
_reflns_number_total             6456
_reflns_number_gt                5559
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    SHELXs-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ?
_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^)+(0.0390P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6456
_refine_ls_number_parameters     309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0741
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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_occupancy
Pd(1) pd -0.0008(1) 0.4473(1) 0.1914(1) 0.015(1) 1
P(1) p 0.2188(1) 0.3589(1) 0.1610(1) 0.014(1) 1
P(2) p 0.1254(1) 0.6381(1) 0.2898(1) 0.017(1) 1
Cl(1) cl -0.2288(1) 0.5193(1) 0.2545(1) 0.027(1) 1
Cl(2) cl -0.1523(1) 0.2721(1) 0.0774(1) 0.027(1) 1
C(1) c 0.2897(3) 0.3460(3) 0.0503(2) 0.018(1) 1
C(2) c 0.2050(3) 0.4165(3) -0.0025(2) 0.024(1) 1
C(3) c 0.4639(3) 0.3815(3) 0.0546(2) 0.022(1) 1
C(4) c 0.2340(3) 0.1941(3) 0.0195(2) 0.020(1) 1
C(5) c 0.3254(4) 0.1035(3) -0.0486(2) 0.031(1) 1
C(6) c 0.2290(3) 0.1757(3) 0.1128(2) 0.019(1) 1
C(7) c 0.0962(3) 0.0775(3) 0.1185(2) 0.025(1) 1
C(8) c 0.3779(3) 0.1358(3) 0.1449(2) 0.025(1) 1
C(9) c 0.2976(3) 0.7563(3) 0.2836(2) 0.025(1) 1
C(10) c 0.4504(3) 0.7661(3) 0.3378(2) 0.034(1) 1
C(11) c 0.3278(4) 0.7428(3) 0.1873(2) 0.033(1) 1
C(12) c 0.2036(4) 0.8710(3) 0.3270(2) 0.039(1) 1
C(13) c 0.2629(6) 0.9730(5) 0.4151(3) 0.039(1) 0.65
C(13') c 0.2327(10) 1.0029(7) 0.3206(7) 0.037(2) 0.35
C(14) c 0.0382(3) 0.7955(3) 0.3136(2) 0.024(1) 1
C(15) c -0.0562(4) 0.8368(3) 0.3937(2) 0.031(1) 1
C(16) c -0.0560(4) 0.8018(3) 0.2317(2) 0.031(1) 1
C(17) c 0.3678(3) 0.4402(3) 0.2541(2) 0.016(1) 1
C(18) c 0.1557(3) 0.6154(3) 0.3971(2) 0.023(1) 1
C(19) c 0.3360(3) 0.4298(3) 0.3445(2) 0.018(1) 1
C(20) c 0.4130(3) 0.3388(3) 0.3695(2) 0.023(1) 1
C(21) c 0.4005(4) 0.3216(3) 0.4507(2) 0.029(1) 1
C(22) c 0.3093(4) 0.3956(3) 0.5107(2) 0.030(1) 1
C(23) c 0.2326(3) 0.4863(3) 0.4879(2) 0.026(1) 1
C(24) c 0.2438(3) 0.5061(3) 0.4058(2) 0.018(1) 1
Cl(3) cl -0.3289(1) 0.0833(1) 0.3169(1) 0.047(1) 1
Cl(4) cl -0.0287(1) 0.2382(1) 0.3495(1) 0.059(1) 1
C(25) c -0.2054(4) 0.1936(4) 0.2841(2) 0.039(1) 1
H(2A) h 0.2326 0.5120 0.0260 0.036 1
H(2B) h 0.0939 0.3940 -0.0035 0.036 1
H(2C h 0.2342 0.3888 -0.0639 0.036 1
H(3A h 0.4916 0.4765 0.0857 0.033 1
H(3B h 0.4954 0.3575 -0.0063 0.033 1
H(3C h 0.5163 0.3332 0.0871 0.033 1
H(4) h 0.1255 0.1793 -0.0080 0.024 1
H(5A h 0.3131 0.1194 -0.1054 0.046 1
H(5B h 0.2873 0.0114 -0.0580 0.046 1
H(5C h 0.4344 0.1216 -0.0261 0.046 1
H(7A h 0.0911 0.0834 0.1810 0.037 1
H(7B h 0.1128 -0.0120 0.0823 0.037 1
H(7C) h -0.0005 0.0981 0.0960 0.037 1
H(8A h 0.4655 0.1981 0.1431 0.038 1
H(8B h 0.3909 0.0469 0.1057 0.038 1
H(8C h 0.3725 0.1368 0.2064 0.038 1
H(10A h 0.5062 0.8548 0.3528 0.051 1
H(10B h 0.5123 0.7010 0.3024 0.051 1
H(10C h 0.4305 0.7490 0.3930 0.051 1
H(11A h 0.3953 0.8205 0.1875 0.049 1
H(11B h 0.2301 0.7356 0.1521 0.049 1
H(11C h 0.3771 0.6636 0.1607 0.049 1
H(13A h 0.3654 1.0141 0.4108 0.058 0.65
H(13B h 0.2692 0.9315 0.4609 0.058 0.65
H(13C h 0.1932 1.0403 0.4316 0.058 0.65
H(13D h 0.1732 1.0629 0.3625 0.056 0.35
H(13E h 0.2019 0.9982 0.2595 0.056 0.35
H(13F h 0.3425 1.0356 0.3356 0.056 0.35
H(15A h 0.0024 0.8329 0.4467 0.046 1
H(15B) h -0.1526 0.7769 0.3811 0.046 1
H(15C) h -0.0790 0.9270 0.4048 0.046 1
H(16A) h -0.0752 0.8928 0.2422 0.046 1
H(16B) h -0.1542 0.7450 0.2214 0.046 1
H(16C h 0.0013 0.7717 0.1790 0.046 1
H(17A h 0.4644 0.4030 0.2372 0.019 1
H(17B h 0.3855 0.5349 0.2614 0.019 1
H(18A h 0.2093 0.6996 0.4399 0.027 1
H(18B h 0.0531 0.6019 0.4177 0.027 1
H(20 h 0.4762 0.2871 0.3289 0.028 1
H(21 h 0.4546 0.2591 0.4654 0.035 1
H(22 h 0.2994 0.3844 0.5668 0.036 1
H(23 h 0.1699 0.5371 0.5293 0.031 1
H(25A) h -0.1882 0.1519 0.2204 0.047 1
H(25B) h -0.2547 0.2737 0.2899 0.047 1

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
Pd(1) 0.011(1) 0.016(1) 0.016(1) 0.002(1) 0.002(1) 0.002(1)
P(1) 0.012(1) 0.015(1) 0.015(1) 0.003(1) 0.003(1) 0.003(1)
P(2) 0.015(1) 0.017(1) 0.017(1) 0.001(1) 0.001(1) 0.003(1)
Cl(1) 0.014(1) 0.028(1) 0.032(1) 0.000(1) 0.007(1) 0.004(1)
Cl(2) 0.018(1) 0.023(1) 0.031(1) -0.003(1) -0.002(1) 0.001(1)
C(1) 0.016(1) 0.022(1) 0.016(1) 0.005(1) 0.004(1) 0.004(1)
C(2) 0.023(1) 0.030(2) 0.018(1) 0.008(1) 0.001(1) 0.003(1)
C(3) 0.017(1) 0.027(2) 0.023(1) 0.010(1) 0.009(1) 0.003(1)
C(4) 0.020(1) 0.021(1) 0.015(1) 0.000(1) 0.003(1) 0.002(1)
C(5) 0.032(2) 0.029(2) 0.026(2) 0.001(1) 0.012(1) 0.006(1)
C(6) 0.018(1) 0.018(1) 0.018(1) 0.002(1) 0.006(1) 0.004(1)
C(7) 0.027(2) 0.017(1) 0.027(2) 0.005(1) 0.007(1) 0.000(1)
C(8) 0.024(1) 0.023(2) 0.028(2) 0.007(1) 0.001(1) 0.007(1)
C(9) 0.021(1) 0.016(1) 0.032(2) 0.002(1) 0.000(1) -0.001(1)
C(10) 0.019(1) 0.028(2) 0.048(2) 0.006(2) -0.002(1) -0.001(1)
C(11) 0.036(2) 0.026(2) 0.040(2) 0.014(2) 0.010(1) 0.002(1)
C(12) 0.027(2) 0.021(2) 0.055(2) -0.005(2) 0.001(2) 0.004(1)
C(13) 0.039(3) 0.025(3) 0.041(3) -0.003(2) 0.007(2) 0.002(2)
C(13') 0.022(4) 0.032(5) 0.059(6) 0.019(5) 0.003(4) 0.005(4)
C(14) 0.022(1) 0.018(1) 0.027(2) 0.000(1) 0.000(1) 0.005(1)
C(15) 0.029(2) 0.024(2) 0.032(2) -0.001(1) 0.004(1) 0.010(1)
C(16) 0.031(2) 0.024(2) 0.037(2) 0.009(1) 0.000(1) 0.009(1)
C(17) 0.014(1) 0.016(1) 0.017(1) 0.003(1) 0.001(1) 0.001(1)
C(18) 0.022(1) 0.026(2) 0.017(1) 0.003(1) 0.003(1) 0.004(1)
C(19) 0.016(1) 0.021(1) 0.016(1) 0.006(1) -0.002(1) -0.003(1)
C(20) 0.025(1) 0.020(2) 0.021(1) 0.003(1) -0.002(1) 0.003(1)
C(21) 0.038(2) 0.024(2) 0.025(2) 0.011(1) -0.009(1) -0.001(1)
C(22) 0.040(2) 0.029(2) 0.020(2) 0.011(1) -0.002(1) -0.008(1)
C(23) 0.028(2) 0.028(2) 0.017(1) 0.004(1) 0.003(1) -0.003(1)
C(24) 0.017(1) 0.020(1) 0.015(1) 0.003(1) -0.001(1) -0.004(1)
Cl(3) 0.030(1) 0.039(1) 0.083(1) 0.034(1) 0.015(1) 0.007(1)
Cl(4) 0.029(1) 0.071(1) 0.050(1) -0.013(1) 0.004(1) -0.009(1)
C(25) 0.028(2) 0.044(2) 0.045(2) 0.018(2) 0.006(2) -0.006(2)

_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
Pd(1) P(1) 2.2474(7)
Pd(1) P(2) 2.2650(7)
Pd(1) Cl(2) 2.3628(7)
Pd(1) Cl(1) 2.3781(7)
P(1) C(17) 1.833(3)
P(1) C(1) 1.870(3)
P(1) C(6) 1.891(3)
P(2) C(18) 1.817(3)
P(2) C(14) 1.876(3)
P(2) C(9) 1.912(3)
C(1) C(2) 1.527(4)
C(1) C(3) 1.531(4)
C(1) C(4) 1.572(4)
C(4) C(5) 1.527(4)
C(4) C(6) 1.568(4)
C(6) C(7) 1.526(4)
C(6) C(8) 1.534(4)
C(9) C(10) 1.530(4)
C(9) C(11) 1.533(4)
C(9) C(12) 1.553(4)
C(12) C(13') 1.468(5)
C(12) C(13) 1.491(4)
C(12) C(14) 1.560(4)
C(14) C(15) 1.526(4)
C(14) C(16) 1.533(4)
C(17) C(19) 1.521(4)
C(18) C(24) 1.522(4)
C(19) C(20) 1.403(4)
C(19) C(24) 1.407(4)
C(20) C(21) 1.377(4)
C(21) C(22) 1.380(5)
C(22) C(23) 1.380(4)
C(23) C(24) 1.403(4)
Cl(3) C(25) 1.762(3)
Cl(4) C(25) 1.749(4)

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
P(1) Pd(1) P(2) 92.36(2)
P(1) Pd(1) Cl(2) 93.79(2)
P(2) Pd(1) Cl(2) 170.03(3)
P(1) Pd(1) Cl(1) 165.17(3)
P(2) Pd(1) Cl(1) 86.67(2)
Cl(2) Pd(1) Cl(1) 89.37(2)
C(17) P(1) C(1) 112.14(12)
C(17) P(1) C(6) 111.20(12)
C(1) P(1) C(6) 79.64(12)
C(17) P(1) Pd(1) 110.00(9)
C(1) P(1) Pd(1) 116.79(9)
C(6) P(1) Pd(1) 123.95(9)
C(18) P(2) C(14) 105.79(13)
C(18) P(2) C(9) 106.21(13)
C(14) P(2) C(9) 78.85(13)
C(18) P(2) Pd(1) 107.62(10)
C(14) P(2) Pd(1) 120.19(9)
C(9) P(2) Pd(1) 133.51(10)
C(2) C(1) C(3) 110.7(2)
C(2) C(1) C(4) 113.5(2)
C(3) C(1) C(4) 114.4(2)
C(2) C(1) P(1) 115.47(19)
C(3) C(1) P(1) 113.86(18)
C(4) C(1) P(1) 87.18(15)
C(5) C(4) C(6) 117.1(2)
C(5) C(4) C(1) 116.7(2)
C(6) C(4) C(1) 100.2(2)
C(7) C(6) C(8) 107.4(2)
C(7) C(6) C(4) 114.9(2)
C(8) C(6) C(4) 113.5(2)
C(7) C(6) P(1) 120.27(19)
C(8) C(6) P(1) 113.18(19)
C(4) C(6) P(1) 86.56(16)
C(10) C(9) C(11) 109.2(3)
C(10) C(9) C(12) 113.3(3)
C(11) C(9) C(12) 112.6(3)
C(10) C(9) P(2) 119.8(2)
C(11) C(9) P(2) 112.9(2)
C(12) C(9) P(2) 87.63(19)
C(13') C(12) C(13) 68.1(5)
C(13') C(12) C(9) 124.4(5)
C(13) C(12) C(9) 119.7(3)
C(13') C(12) C(14) 122.2(4)
C(13) C(12) C(14) 120.2(3)
C(9) C(12) C(14) 101.3(2)
C(15) C(14) C(16) 108.5(2)
C(15) C(14) C(12) 115.9(3)
C(16) C(14) C(12) 112.0(3)
C(15) C(14) P(2) 118.1(2)
C(16) C(14) P(2) 112.7(2)
C(12) C(14) P(2) 88.69(18)
C(19) C(17) P(1) 116.82(18)
C(24) C(18) P(2) 120.64(19)
C(20) C(19) C(24) 117.8(2)
C(20) C(19) C(17) 115.7(2)
C(24) C(19) C(17) 126.4(2)
C(21) C(20) C(19) 122.5(3)
C(20) C(21) C(22) 119.7(3)
C(21) C(22) C(23) 119.0(3)
C(22) C(23) C(24) 122.5(3)
C(23) C(24) C(19) 118.5(3)
C(23) C(24) C(18) 113.3(2)
C(19) C(24) C(18) 128.1(2)
Cl(4) C(25) Cl(3) 111.4(2)

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.152

# Attachment 'Compound 12.CIF'

data_compound12
_database_code_depnum_ccdc_archive 'CCDC 756180'
#TrackingRef 'Compound 12.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H40 Mo O4 P2'
_chemical_formula_sum            'C28 H40 Mo O4 P2'
_chemical_formula_weight         598.48

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           Monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   37.8437(7)
_cell_length_b                   8.7185(2)
_cell_length_c                   18.4939(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.0023(10)
_cell_angle_gamma                90.00
_cell_volume                     5769.4(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4918
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      27.45

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2496
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8801
_exptl_absorpt_correction_T_max  0.9003
_exptl_absorpt_process_details   Denzo/Scalepack

_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  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26788
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.45
_reflns_number_total             6561
_reflns_number_gt                4918
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    SHELXs-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ?
_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^)+(0.0390P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6561
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0915
_refine_ls_wR_factor_gt          0.0836
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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
Mo1 Mo 0.116647(7) 0.45153(2) 0.089004(12) 0.02052(8) Uani 1 1 d . . .
P1 P 0.16801(2) 0.60379(7) 0.05908(4) 0.01949(16) Uani 1 1 d . . .
P2 P 0.09275(2) 0.70506(7) 0.12540(4) 0.01886(16) Uani 1 1 d . . .
O4 O 0.05795(7) 0.4528(2) -0.07984(12) 0.0468(6) Uani 1 1 d . . .
O1 O 0.13663(8) 0.1472(2) 0.02217(17) 0.0707(9) Uani 1 1 d . . .
O2 O 0.16712(7) 0.3387(2) 0.25285(12) 0.0473(6) Uani 1 1 d . . .
O3 O 0.05645(6) 0.2331(2) 0.11663(11) 0.0359(5) Uani 1 1 d . . .
C4 C 0.07964(9) 0.4684(3) -0.02026(17) 0.0297(7) Uani 1 1 d . . .
C1 C 0.13128(9) 0.2612(3) 0.04897(18) 0.0394(8) Uani 1 1 d . . .
C2 C 0.14973(9) 0.3897(3) 0.19465(17) 0.0320(7) Uani 1 1 d . . .
C3 C 0.07776(8) 0.3201(3) 0.10843(15) 0.0260(6) Uani 1 1 d . . .
C5 C 0.15203(8) 0.7683(3) -0.00829(15) 0.0266(6) Uani 1 1 d . . .
H5A H 0.1581 0.8643 0.0218 0.032 Uiso 1 1 calc R . .
H5B H 0.1668 0.7679 -0.0437 0.032 Uiso 1 1 calc R . .
C6 C 0.11135(8) 0.7734(2) -0.05541(14) 0.0214(6) Uani 1 1 d . . .
C7 C 0.10061(9) 0.7401(3) -0.13347(15) 0.0294(7) Uani 1 1 d . . .
H7 H 0.1191 0.7104 -0.1553 0.035 Uiso 1 1 calc R . .
C8 C 0.06361(10) 0.7493(3) -0.17989(15) 0.0346(7) Uani 1 1 d . . .
H8 H 0.0569 0.7252 -0.2328 0.042 Uiso 1 1 calc R . .
C9 C 0.03654(9) 0.7938(3) -0.14864(16) 0.0349(7) Uani 1 1 d . . .
H9 H 0.0110 0.7992 -0.1797 0.042 Uiso 1 1 calc R . .
C10 C 0.04700(8) 0.8301(3) -0.07172(14) 0.0254(6) Uani 1 1 d . . .
H10 H 0.0284 0.8627 -0.0507 0.030 Uiso 1 1 calc R . .
C11 C 0.08379(7) 0.8204(2) -0.02445(13) 0.0189(5) Uani 1 1 d . . .
C12 C 0.09358(8) 0.8646(2) 0.05944(13) 0.0215(6) Uani 1 1 d . . .
H12A H 0.0758 0.9446 0.0639 0.026 Uiso 1 1 calc R . .
H12B H 0.1189 0.9106 0.0765 0.026 Uiso 1 1 calc R . .
C13 C 0.21302(8) 0.6851(3) 0.12828(15) 0.0276(6) Uani 1 1 d . . .
C16 C 0.22326(10) 0.6082(4) 0.20701(16) 0.0498(9) Uani 1 1 d . . .
H16A H 0.2489 0.6364 0.2375 0.075 Uiso 1 1 calc R . .
H16B H 0.2215 0.4966 0.2006 0.075 Uiso 1 1 calc R . .
H16C H 0.2060 0.6426 0.2332 0.075 Uiso 1 1 calc R . .
C17 C 0.21739(10) 0.8593(3) 0.14013(17) 0.0419(8) Uani 1 1 d . . .
H17A H 0.1998 0.8961 0.1652 0.063 Uiso 1 1 calc R . .
H17B H 0.2121 0.9101 0.0905 0.063 Uiso 1 1 calc R . .
H17C H 0.2430 0.8829 0.1723 0.063 Uiso 1 1 calc R . .
C14 C 0.23492(8) 0.6242(3) 0.07612(15) 0.0287(6) Uani 1 1 d . . .
H14 H 0.2360 0.7094 0.0407 0.034 Uiso 1 1 calc R . .
C18 C 0.27485(9) 0.5683(4) 0.1141(2) 0.0464(8) Uani 1 1 d . . .
H18A H 0.2906 0.6544 0.1401 0.070 Uiso 1 1 calc R . .
H18B H 0.2846 0.5263 0.0752 0.070 Uiso 1 1 calc R . .
H18C H 0.2751 0.4884 0.1516 0.070 Uiso 1 1 calc R . .
C15 C 0.20574(8) 0.5046(3) 0.02823(16) 0.0261(6) Uani 1 1 d . . .
C19 C 0.21318(9) 0.3411(3) 0.0589(2) 0.0470(9) Uani 1 1 d . . .
H19A H 0.1947 0.2717 0.0253 0.071 Uiso 1 1 calc R . .
H19B H 0.2113 0.3370 0.1105 0.071 Uiso 1 1 calc R . .
H19C H 0.2383 0.3097 0.0607 0.071 Uiso 1 1 calc R . .
C20 C 0.20149(10) 0.5037(4) -0.05603(18) 0.0454(8) Uani 1 1 d . . .
H20A H 0.2239 0.4587 -0.0631 0.068 Uiso 1 1 calc R . .
H20B H 0.1983 0.6091 -0.0755 0.068 Uiso 1 1 calc R . .
H20C H 0.1795 0.4427 -0.0840 0.068 Uiso 1 1 calc R . .
C21 C 0.04751(8) 0.7302(3) 0.14774(14) 0.0232(6) Uani 1 1 d . . .
C24 C 0.03532(9) 0.5796(3) 0.17392(18) 0.0359(7) Uani 1 1 d . . .
H24A H 0.0159 0.5997 0.1972 0.054 Uiso 1 1 calc R . .
H24B H 0.0568 0.5307 0.2116 0.054 Uiso 1 1 calc R . .
H24C H 0.0253 0.5114 0.1298 0.054 Uiso 1 1 calc R . .
C25 C 0.01408(8) 0.8018(3) 0.08791(16) 0.0322(7) Uani 1 1 d . . .
H25A H 0.0052 0.7331 0.0437 0.048 Uiso 1 1 calc R . .
H25B H 0.0214 0.9004 0.0716 0.048 Uiso 1 1 calc R . .
H25C H -0.0060 0.8183 0.1098 0.048 Uiso 1 1 calc R . .
C22 C 0.06821(8) 0.8423(3) 0.21406(15) 0.0278(6) Uani 1 1 d . . .
H22 H 0.0633 0.9487 0.1930 0.033 Uiso 1 1 calc R . .
C26 C 0.05767(9) 0.8390(3) 0.28661(16) 0.0382(8) Uani 1 1 d . . .
H26A H 0.0603 0.7343 0.3070 0.057 Uiso 1 1 calc R . .
H26B H 0.0317 0.8726 0.2750 0.057 Uiso 1 1 calc R . .
H26C H 0.0742 0.9079 0.3247 0.057 Uiso 1 1 calc R . .
C23 C 0.10932(8) 0.8036(3) 0.22220(14) 0.0258(6) Uani 1 1 d . . .
C28 C 0.12820(10) 0.6899(3) 0.28639(15) 0.0396(8) Uani 1 1 d . . .
H28A H 0.1530 0.6632 0.2842 0.059 Uiso 1 1 calc R . .
H28B H 0.1129 0.5970 0.2800 0.059 Uiso 1 1 calc R . .
H28C H 0.1308 0.7369 0.3360 0.059 Uiso 1 1 calc R . .
C27 C 0.13414(9) 0.9464(3) 0.23230(16) 0.0359(7) Uani 1 1 d . . .
H27A H 0.1366 0.9949 0.2815 0.054 Uiso 1 1 calc R . .
H27B H 0.1228 1.0190 0.1908 0.054 Uiso 1 1 calc R . .
H27C H 0.1589 0.9165 0.2311 0.054 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.02491(15) 0.01377(12) 0.02627(14) 0.00324(8) 0.01300(11) 0.00151(9)
P1 0.0208(4) 0.0168(3) 0.0216(3) 0.0000(2) 0.0079(3) 0.0005(3)
P2 0.0220(4) 0.0156(3) 0.0204(3) 0.0021(2) 0.0088(3) 0.0011(3)
O4 0.0636(18) 0.0369(12) 0.0304(12) -0.0035(9) 0.0022(12) -0.0199(11)
O1 0.072(2) 0.0225(11) 0.147(3) -0.0216(13) 0.077(2) -0.0115(11)
O2 0.0469(16) 0.0489(13) 0.0422(13) 0.0211(10) 0.0090(12) 0.0074(11)
O3 0.0398(14) 0.0266(10) 0.0489(13) 0.0032(9) 0.0249(11) -0.0072(9)
C4 0.041(2) 0.0159(13) 0.0352(17) -0.0002(11) 0.0167(15) -0.0085(12)
C1 0.046(2) 0.0189(14) 0.069(2) 0.0012(13) 0.0389(19) -0.0034(13)
C2 0.0324(19) 0.0289(14) 0.0367(17) 0.0087(13) 0.0141(15) 0.0025(13)
C3 0.0343(19) 0.0175(12) 0.0307(15) 0.0029(11) 0.0169(13) 0.0040(12)
C5 0.0235(17) 0.0236(13) 0.0379(16) 0.0101(11) 0.0169(13) 0.0016(11)
C6 0.0264(17) 0.0148(12) 0.0239(13) 0.0070(10) 0.0096(12) 0.0023(10)
C7 0.046(2) 0.0229(13) 0.0262(15) 0.0081(11) 0.0214(15) 0.0071(12)
C8 0.053(2) 0.0276(14) 0.0196(14) -0.0005(11) 0.0069(15) 0.0016(14)
C9 0.034(2) 0.0370(15) 0.0270(16) 0.0046(12) 0.0004(14) -0.0031(13)
C10 0.0234(17) 0.0273(13) 0.0252(14) 0.0068(11) 0.0077(12) 0.0049(11)
C11 0.0247(16) 0.0118(11) 0.0208(13) 0.0049(9) 0.0082(12) 0.0019(10)
C12 0.0286(17) 0.0157(12) 0.0224(13) 0.0013(10) 0.0115(12) 0.0008(10)
C13 0.0263(17) 0.0294(14) 0.0253(14) -0.0031(11) 0.0058(13) -0.0063(12)
C16 0.045(2) 0.071(2) 0.0239(16) 0.0057(15) -0.0016(15) -0.0176(18)
C17 0.043(2) 0.0397(17) 0.0465(19) -0.0185(14) 0.0195(17) -0.0164(15)
C14 0.0243(17) 0.0281(14) 0.0320(15) -0.0007(11) 0.0068(13) -0.0034(12)
C18 0.0232(19) 0.0485(19) 0.061(2) 0.0040(15) 0.0040(17) -0.0013(15)
C15 0.0186(16) 0.0241(12) 0.0375(16) -0.0051(11) 0.0119(13) -0.0001(11)
C19 0.030(2) 0.0245(15) 0.090(3) -0.0024(15) 0.0247(19) 0.0064(13)
C20 0.041(2) 0.0541(18) 0.048(2) -0.0263(16) 0.0238(17) -0.0113(16)
C21 0.0250(17) 0.0196(12) 0.0295(15) 0.0018(10) 0.0151(13) 0.0011(11)
C24 0.036(2) 0.0291(14) 0.053(2) 0.0038(13) 0.0284(17) -0.0004(13)
C25 0.0276(18) 0.0353(15) 0.0384(17) 0.0037(12) 0.0171(14) 0.0039(13)
C22 0.0339(19) 0.0235(13) 0.0287(15) 0.0041(11) 0.0141(13) 0.0061(12)
C26 0.044(2) 0.0400(16) 0.0386(17) -0.0030(13) 0.0241(16) 0.0047(14)
C23 0.0292(18) 0.0279(13) 0.0211(13) 0.0005(10) 0.0090(12) 0.0075(12)
C28 0.050(2) 0.0465(17) 0.0226(15) 0.0064(13) 0.0117(15) 0.0203(15)
C27 0.036(2) 0.0401(16) 0.0312(16) -0.0142(12) 0.0106(15) -0.0046(14)

_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
Mo1 C1 1.968(3) . ?
Mo1 C3 1.988(3) . ?
Mo1 C2 2.021(3) . ?
Mo1 C4 2.055(3) . ?
Mo1 P1 2.5588(7) . ?
Mo1 P2 2.5599(6) . ?
P1 C5 1.867(2) . ?
P1 C13 1.903(3) . ?
P1 C15 1.908(3) . ?
P2 C12 1.857(2) . ?
P2 C23 1.899(3) . ?
P2 C21 1.900(3) . ?
O4 C4 1.148(3) . ?
O1 C1 1.158(3) . ?
O2 C2 1.152(3) . ?
O3 C3 1.153(3) . ?
C5 C6 1.502(4) . ?
C6 C7 1.397(3) . ?
C6 C11 1.405(3) . ?
C7 C8 1.386(4) . ?
C8 C9 1.386(4) . ?
C9 C10 1.384(4) . ?
C10 C11 1.385(4) . ?
C11 C12 1.523(3) . ?
C13 C16 1.534(4) . ?
C13 C17 1.536(4) . ?
C13 C14 1.556(4) . ?
C14 C18 1.524(4) . ?
C14 C15 1.567(4) . ?
C15 C20 1.514(4) . ?
C15 C19 1.526(4) . ?
C21 C25 1.518(4) . ?
C21 C24 1.522(3) . ?
C21 C22 1.565(4) . ?
C22 C26 1.519(4) . ?
C22 C23 1.550(4) . ?
C23 C28 1.533(3) . ?
C23 C27 1.534(4) . ?

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
C1 Mo1 C3 84.13(11) . . ?
C1 Mo1 C2 88.68(12) . . ?
C3 Mo1 C2 86.19(11) . . ?
C1 Mo1 C4 82.86(12) . . ?
C3 Mo1 C4 84.92(11) . . ?
C2 Mo1 C4 168.30(10) . . ?
C1 Mo1 P1 91.69(8) . . ?
C3 Mo1 P1 175.79(7) . . ?
C2 Mo1 P1 94.15(8) . . ?
C4 Mo1 P1 94.16(8) . . ?
C1 Mo1 P2 173.44(10) . . ?
C3 Mo1 P2 95.99(7) . . ?
C2 Mo1 P2 97.88(8) . . ?
C4 Mo1 P2 90.61(7) . . ?
P1 Mo1 P2 88.12(2) . . ?
C5 P1 C13 100.78(12) . . ?
C5 P1 C15 105.07(12) . . ?
C13 P1 C15 77.12(12) . . ?
C5 P1 Mo1 116.05(9) . . ?
C13 P1 Mo1 128.64(9) . . ?
C15 P1 Mo1 121.63(8) . . ?
C12 P2 C23 102.09(11) . . ?
C12 P2 C21 105.41(12) . . ?
C23 P2 C21 77.71(12) . . ?
C12 P2 Mo1 113.01(8) . . ?
C23 P2 Mo1 127.03(8) . . ?
C21 P2 Mo1 125.25(8) . . ?
O4 C4 Mo1 168.7(2) . . ?
O1 C1 Mo1 174.1(3) . . ?
O2 C2 Mo1 172.6(2) . . ?
O3 C3 Mo1 173.7(2) . . ?
C6 C5 P1 117.26(17) . . ?
C7 C6 C11 118.5(3) . . ?
C7 C6 C5 119.5(2) . . ?
C11 C6 C5 121.9(2) . . ?
C8 C7 C6 121.6(3) . . ?
C9 C8 C7 119.5(3) . . ?
C10 C9 C8 119.3(3) . . ?
C9 C10 C11 121.8(3) . . ?
C10 C11 C6 119.2(2) . . ?
C10 C11 C12 119.3(2) . . ?
C6 C11 C12 121.5(2) . . ?
C11 C12 P2 115.44(15) . . ?
C16 C13 C17 108.3(2) . . ?
C16 C13 C14 114.7(3) . . ?
C17 C13 C14 111.8(2) . . ?
C16 C13 P1 111.7(2) . . ?
C17 C13 P1 119.7(2) . . ?
C14 C13 P1 89.80(16) . . ?
C18 C14 C13 118.1(2) . . ?
C18 C14 C15 117.3(2) . . ?
C13 C14 C15 99.1(2) . . ?
C20 C15 C19 108.8(2) . . ?
C20 C15 C14 113.9(2) . . ?
C19 C15 C14 113.6(2) . . ?
C20 C15 P1 118.1(2) . . ?
C19 C15 P1 112.2(2) . . ?
C14 C15 P1 89.29(16) . . ?
C25 C21 C24 108.6(2) . . ?
C25 C21 C22 113.6(2) . . ?
C24 C21 C22 114.6(2) . . ?
C25 C21 P2 119.02(18) . . ?
C24 C21 P2 110.96(18) . . ?
C22 C21 P2 89.19(17) . . ?
C26 C22 C23 117.0(2) . . ?
C26 C22 C21 118.1(2) . . ?
C23 C22 C21 99.8(2) . . ?
C28 C23 C27 108.5(2) . . ?
C28 C23 C22 114.6(2) . . ?
C27 C23 C22 113.0(2) . . ?
C28 C23 P2 111.41(17) . . ?
C27 C23 P2 118.90(19) . . ?
C22 C23 P2 89.66(17) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.152