# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_d:\21js00

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H24 N2 P2'
_chemical_formula_weight         414.40

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

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                   14.4930(3)
_cell_length_b                   10.3290(8)
_cell_length_c                   15.3920(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.523(2)
_cell_angle_gamma                90.00
_cell_volume                     2171.68(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    33528
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      28.59

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Low data completion ratio is due to the limitations of the instrument available
at the Australian Synchrotron operating under rotation data collection with a
fixed detector and affects some high angle data. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'synchrotron BM'
_diffrn_radiation_monochromator  Si<111>
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35591
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         28.59
_reflns_number_total             5447
_reflns_number_gt                5163
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       BLU-ICE
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)' 
;
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The NH was clearly visable in difference maps, located and refined in x,y,z.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0500P)²+1.2285P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5447
_refine_ls_number_parameters     266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0947
_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
P1 P 0.27833(2) 0.36586(3) -0.005954(19) 0.01528(8) Uani 1 1 d . . .
P2 P 0.40996(2) 0.31267(3) 0.192446(19) 0.01549(8) Uani 1 1 d . . .
N1 N 0.38094(7) 0.30230(9) 0.07513(7) 0.01610(19) Uani 1 1 d . . .
N2 N 0.45472(7) 0.25211(10) 0.04019(7) 0.0183(2) Uani 1 1 d . . .
C1 C 0.17687(8) 0.29819(11) 0.02435(8) 0.0163(2) Uani 1 1 d . . .
C2 C 0.18414(9) 0.17988(11) 0.07012(8) 0.0203(2) Uani 1 1 d . . .
H2 H 0.2460 0.1385 0.0944 0.024 Uiso 1 1 calc R . .
C3 C 0.10168(10) 0.12193(13) 0.08061(9) 0.0253(3) Uani 1 1 d . . .
H3 H 0.1077 0.0424 0.1131 0.030 Uiso 1 1 calc R . .
C4 C 0.01061(10) 0.18055(13) 0.04350(10) 0.0263(3) Uani 1 1 d . . .
H4 H -0.0458 0.1407 0.0499 0.032 Uiso 1 1 calc R . .
C5 C 0.00229(9) 0.29746(13) -0.00300(9) 0.0239(2) Uani 1 1 d . . .
H5 H -0.0600 0.3374 -0.0285 0.029 Uiso 1 1 calc R . .
C6 C 0.08454(9) 0.35640(12) -0.01251(8) 0.0194(2) Uani 1 1 d . . .
H6 H 0.0782 0.4366 -0.0442 0.023 Uiso 1 1 calc R . .
C7 C 0.28029(8) 0.53606(11) 0.02826(8) 0.0174(2) Uani 1 1 d . . .
C8 C 0.25963(9) 0.57948(12) 0.10563(9) 0.0207(2) Uani 1 1 d . . .
H8 H 0.2371 0.5201 0.1412 0.025 Uiso 1 1 calc R . .
C9 C 0.27188(10) 0.70948(13) 0.13089(9) 0.0257(3) Uani 1 1 d . . .
H9 H 0.2575 0.7386 0.1835 0.031 Uiso 1 1 calc R . .
C10 C 0.30515(10) 0.79659(12) 0.07930(10) 0.0262(3) Uani 1 1 d . . .
H10 H 0.3138 0.8851 0.0969 0.031 Uiso 1 1 calc R . .
H2N H 0.4673(13) 0.3139(17) 0.0041(12) 0.030 Uiso 1 1 d . . .
C11 C 0.32572(9) 0.75473(12) 0.00223(9) 0.0238(2) Uani 1 1 d . . .
H11 H 0.3487 0.8144 -0.0328 0.029 Uiso 1 1 calc R . .
C12 C 0.31263(9) 0.62507(12) -0.02383(8) 0.0206(2) Uani 1 1 d . . .
H12 H 0.3257 0.5969 -0.0773 0.025 Uiso 1 1 calc R . .
C13 C 0.51770(8) 0.41780(11) 0.22853(8) 0.0167(2) Uani 1 1 d . . .
C14 C 0.53461(9) 0.51097(12) 0.17009(8) 0.0209(2) Uani 1 1 d . . .
H14 H 0.4927 0.5154 0.1077 0.025 Uiso 1 1 calc R . .
C15 C 0.61203(10) 0.59749(13) 0.20180(9) 0.0243(2) Uani 1 1 d . . .
H15 H 0.6228 0.6604 0.1612 0.029 Uiso 1 1 calc R . .
C16 C 0.67380(9) 0.59221(13) 0.29292(9) 0.0224(2) Uani 1 1 d . . .
H16 H 0.7273 0.6506 0.3145 0.027 Uiso 1 1 calc R . .
C17 C 0.65692(9) 0.50124(13) 0.35209(9) 0.0234(2) Uani 1 1 d . . .
H17 H 0.6985 0.4980 0.4146 0.028 Uiso 1 1 calc R . .
C18 C 0.57949(9) 0.41471(12) 0.32042(8) 0.0219(2) Uani 1 1 d . . .
H18 H 0.5684 0.3529 0.3616 0.026 Uiso 1 1 calc R . .
C19 C 0.46546(8) 0.15404(11) 0.23057(8) 0.0175(2) Uani 1 1 d . . .
C20 C 0.40875(9) 0.06445(12) 0.25859(8) 0.0193(2) Uani 1 1 d . . .
H20 H 0.3453 0.0884 0.2581 0.023 Uiso 1 1 calc R . .
C21 C 0.44381(10) -0.05924(12) 0.28716(8) 0.0239(3) Uani 1 1 d . . .
H21 H 0.4045 -0.1192 0.3060 0.029 Uiso 1 1 calc R . .
C22 C 0.53647(11) -0.09480(13) 0.28804(9) 0.0269(3) Uani 1 1 d . . .
H22 H 0.5606 -0.1793 0.3072 0.032 Uiso 1 1 calc R . .
C23 C 0.59402(10) -0.00640(13) 0.26082(9) 0.0265(3) Uani 1 1 d . . .
H23 H 0.6574 -0.0308 0.2614 0.032 Uiso 1 1 calc R . .
C24 C 0.55913(9) 0.11759(13) 0.23274(9) 0.0225(2) Uani 1 1 d . . .
H24 H 0.5991 0.1777 0.2150 0.027 Uiso 1 1 calc R . .
C25 C 0.41890(10) 0.13691(12) -0.01580(10) 0.0250(3) Uani 1 1 d . . .
H25A H 0.4127 0.0656 0.0239 0.037 Uiso 1 1 calc R . .
H25B H 0.4652 0.1125 -0.0471 0.037 Uiso 1 1 calc R . .
H25C H 0.3548 0.1553 -0.0618 0.037 Uiso 1 1 calc R . .


_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 N1 1.7204(10) . ?
P1 C1 1.8239(12) . ?
P1 C7 1.8326(12) . ?
P2 N1 1.7150(10) . ?
P2 C13 1.8292(12) . ?
P2 C19 1.8331(12) . ?
N1 N2 1.4443(13) . ?
N2 C25 1.4591(16) . ?
N2 H2N 0.903(18) . ?
C1 C2 1.3968(16) . ?
C1 C6 1.4024(16) . ?
C2 C3 1.3935(17) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3890(17) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.3955(16) . ?
C7 C12 1.3996(16) . ?
C8 C9 1.3927(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.3887(19) . ?
C9 H9 0.9500 . ?
C10 C11 1.3854(19) . ?
C10 H10 0.9500 . ?
C11 C12 1.3927(18) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.3939(16) . ?
C13 C18 1.3990(16) . ?
C14 C15 1.3892(17) . ?
C14 H14 0.9500 . ?
C15 C16 1.3900(17) . ?
C15 H15 0.9500 . ?
C16 C17 1.3861(18) . ?
C16 H16 0.9500 . ?
C17 C18 1.3892(18) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.3981(16) . ?
C19 C24 1.3985(16) . ?
C20 C21 1.3908(17) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.392(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3915(17) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 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
N1 P1 C1 104.10(5) . . ?
N1 P1 C7 103.35(5) . . ?
C1 P1 C7 103.33(5) . . ?
N1 P2 C13 103.93(5) . . ?
N1 P2 C19 102.02(5) . . ?
C13 P2 C19 101.23(5) . . ?
N2 N1 P2 117.58(7) . . ?
N2 N1 P1 115.78(7) . . ?
P2 N1 P1 126.04(6) . . ?
N1 N2 C25 110.56(9) . . ?
N1 N2 H2N 107.6(11) . . ?
C25 N2 H2N 108.5(11) . . ?
C2 C1 C6 118.69(11) . . ?
C2 C1 P1 122.20(9) . . ?
C6 C1 P1 118.30(9) . . ?
C3 C2 C1 120.75(12) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C4 C3 C2 119.92(12) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 119.86(12) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.39(12) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 120.39(12) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
C8 C7 C12 119.09(11) . . ?
C8 C7 P1 124.50(9) . . ?
C12 C7 P1 116.20(9) . . ?
C9 C8 C7 120.29(12) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 120.08(12) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 120.17(12) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 119.95(12) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C7 120.41(12) . . ?
C11 C12 H12 119.8 . . ?
C7 C12 H12 119.8 . . ?
C14 C13 C18 118.49(11) . . ?
C14 C13 P2 122.03(9) . . ?
C18 C13 P2 119.11(9) . . ?
C15 C14 C13 120.86(11) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 120.10(11) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 119.60(11) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 120.32(11) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C13 120.61(11) . . ?
C17 C18 H18 119.7 . . ?
C13 C18 H18 119.7 . . ?
C20 C19 C24 118.71(11) . . ?
C20 C19 P2 116.75(9) . . ?
C24 C19 P2 124.54(9) . . ?
C21 C20 C19 121.02(11) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C22 C21 C20 119.75(12) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 119.89(12) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C24 C23 C22 120.34(12) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C19 120.28(12) . . ?
C23 C24 H24 119.9 . . ?
C19 C24 H24 119.9 . . ?
N2 C25 H25A 109.5 . . ?
N2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

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
C13 P2 N1 N2 58.59(9) . . . . ?
C19 P2 N1 N2 -46.36(9) . . . . ?
C13 P2 N1 P1 -112.10(7) . . . . ?
C19 P2 N1 P1 142.95(7) . . . . ?
C1 P1 N1 N2 134.51(8) . . . . ?
C7 P1 N1 N2 -117.80(8) . . . . ?
C1 P1 N1 P2 -54.65(8) . . . . ?
C7 P1 N1 P2 53.04(8) . . . . ?
P2 N1 N2 C25 120.71(9) . . . . ?
P1 N1 N2 C25 -67.65(11) . . . . ?
N1 P1 C1 C2 -27.09(11) . . . . ?
C7 P1 C1 C2 -134.79(10) . . . . ?
N1 P1 C1 C6 163.38(9) . . . . ?
C7 P1 C1 C6 55.67(10) . . . . ?
C6 C1 C2 C3 -1.25(17) . . . . ?
P1 C1 C2 C3 -170.75(10) . . . . ?
C1 C2 C3 C4 1.45(19) . . . . ?
C2 C3 C4 C5 -0.7(2) . . . . ?
C3 C4 C5 C6 -0.14(19) . . . . ?
C4 C5 C6 C1 0.32(19) . . . . ?
C2 C1 C6 C5 0.37(17) . . . . ?
P1 C1 C6 C5 170.28(9) . . . . ?
N1 P1 C7 C8 -72.04(11) . . . . ?
C1 P1 C7 C8 36.23(11) . . . . ?
N1 P1 C7 C12 102.60(9) . . . . ?
C1 P1 C7 C12 -149.13(9) . . . . ?
C12 C7 C8 C9 -0.52(18) . . . . ?
P1 C7 C8 C9 173.98(10) . . . . ?
C7 C8 C9 C10 -0.3(2) . . . . ?
C8 C9 C10 C11 0.4(2) . . . . ?
C9 C10 C11 C12 0.3(2) . . . . ?
C10 C11 C12 C7 -1.05(19) . . . . ?
C8 C7 C12 C11 1.17(17) . . . . ?
P1 C7 C12 C11 -173.77(9) . . . . ?
N1 P2 C13 C14 27.49(11) . . . . ?
C19 P2 C13 C14 133.03(10) . . . . ?
N1 P2 C13 C18 -159.61(9) . . . . ?
C19 P2 C13 C18 -54.07(11) . . . . ?
C18 C13 C14 C15 1.08(18) . . . . ?
P2 C13 C14 C15 174.02(10) . . . . ?
C13 C14 C15 C16 -0.1(2) . . . . ?
C14 C15 C16 C17 -0.8(2) . . . . ?
C15 C16 C17 C18 0.8(2) . . . . ?
C16 C17 C18 C13 0.2(2) . . . . ?
C14 C13 C18 C17 -1.10(18) . . . . ?
P2 C13 C18 C17 -174.25(10) . . . . ?
N1 P2 C19 C20 -105.07(9) . . . . ?
C13 P2 C19 C20 147.87(9) . . . . ?
N1 P2 C19 C24 74.51(11) . . . . ?
C13 P2 C19 C24 -32.55(12) . . . . ?
C24 C19 C20 C21 -0.73(17) . . . . ?
P2 C19 C20 C21 178.88(9) . . . . ?
C19 C20 C21 C22 0.01(18) . . . . ?
C20 C21 C22 C23 0.34(19) . . . . ?
C21 C22 C23 C24 0.0(2) . . . . ?
C22 C23 C24 C19 -0.8(2) . . . . ?
C20 C19 C24 C23 1.09(18) . . . . ?
P2 C19 C24 C23 -178.48(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        28.59
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.056
_database_code_depnum_ccdc_archive 'CCDC 995241'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_d:\21js1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H38 N2 P2'
_chemical_formula_weight         512.58

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'
N N 0.0061 0.0033 '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
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   10.2160(7)
_cell_length_b                   10.3180(3)
_cell_length_c                   14.3790(6)
_cell_angle_alpha                79.664(2)
_cell_angle_beta                 76.635(2)
_cell_angle_gamma                71.842(5)
_cell_volume                     1391.70(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22097
_cell_measurement_theta_min      1.47
_cell_measurement_theta_max      28.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Low data completion ratio is due to the limitations of the instrument available
at the Australian Synchrotron operating under rotation data collection with a
fixed detector and affects some high angle data. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71085
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'synchrotron BM'
_diffrn_radiation_monochromator  Si<111>
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23874
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         28.56
_reflns_number_total             6344
_reflns_number_gt                5917
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       BLU-ICE
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)' 
;
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0552P)²+0.6687P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6344
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1072
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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 0.69084(3) 0.61882(3) 0.19648(2) 0.01203(9) Uani 1 1 d . . .
P2 P 0.79329(3) 0.86234(3) 0.09389(2) 0.01277(9) Uani 1 1 d . . .
N1 N 0.71010(11) 0.77844(10) 0.19279(7) 0.0128(2) Uani 1 1 d . . .
N2 N 0.72802(11) 0.96597(11) 0.39185(7) 0.0135(2) Uani 1 1 d . . .
C25 C 0.66330(12) 0.85470(12) 0.27854(9) 0.0136(2) Uani 1 1 d . . .
H25A H 0.6074 0.8058 0.3301 0.016 Uiso 1 1 calc R . .
H25B H 0.6012 0.9469 0.2615 0.016 Uiso 1 1 calc R . .
C1 C 0.50072(12) 0.64420(13) 0.23165(9) 0.0143(2) Uani 1 1 d . . .
C7 C 0.75172(12) 0.53147(12) 0.30871(9) 0.0134(2) Uani 1 1 d . . .
C9 C 0.95265(14) 0.44179(14) 0.38823(10) 0.0199(3) Uani 1 1 d . . .
H9 H 1.0492 0.4289 0.3872 0.024 Uiso 1 1 calc R . .
C13 C 0.74084(13) 0.82279(13) -0.00877(9) 0.0139(2) Uani 1 1 d . . .
C27 C 0.76331(13) 1.09764(13) 0.36037(10) 0.0169(2) Uani 1 1 d . . .
H27 H 0.7150 1.1573 0.4130 0.020 Uiso 1 1 calc R . .
C12 C 0.67013(13) 0.48228(13) 0.39136(9) 0.0169(2) Uani 1 1 d . . .
H12 H 0.5733 0.4956 0.3930 0.020 Uiso 1 1 calc R . .
C19 C 0.97996(12) 0.76768(13) 0.07426(9) 0.0143(2) Uani 1 1 d . . .
C11 C 0.72855(14) 0.41404(14) 0.47123(9) 0.0196(3) Uani 1 1 d . . .
H11 H 0.6716 0.3809 0.5267 0.023 Uiso 1 1 calc R . .
C17 C 0.55579(14) 0.82308(15) -0.08910(10) 0.0204(3) Uani 1 1 d . . .
H17 H 0.4601 0.8300 -0.0865 0.025 Uiso 1 1 calc R . .
C8 C 0.89503(13) 0.50786(13) 0.30818(10) 0.0171(2) Uani 1 1 d . . .
H8 H 0.9532 0.5377 0.2521 0.021 Uiso 1 1 calc R . .
C21 C 1.21780(14) 0.78465(15) 0.04614(10) 0.0209(3) Uani 1 1 d . . .
H21 H 1.2803 0.8379 0.0420 0.025 Uiso 1 1 calc R . .
C20 C 1.07343(14) 0.84392(14) 0.06866(9) 0.0171(2) Uani 1 1 d . . .
H20 H 1.0382 0.9374 0.0803 0.020 Uiso 1 1 calc R . .
C2 C 0.40223(13) 0.77083(13) 0.24663(9) 0.0169(2) Uani 1 1 d . . .
H2 H 0.4330 0.8502 0.2413 0.020 Uiso 1 1 calc R . .
C10 C 0.86979(14) 0.39410(14) 0.47022(10) 0.0196(3) Uani 1 1 d . . .
H10 H 0.9095 0.3483 0.5250 0.023 Uiso 1 1 calc R . .
C18 C 0.60020(13) 0.83344(14) -0.00672(9) 0.0175(2) Uani 1 1 d . . .
H18 H 0.5341 0.8479 0.0516 0.021 Uiso 1 1 calc R . .
C15 C 0.79093(14) 0.79211(15) -0.17842(9) 0.0212(3) Uani 1 1 d . . .
H15 H 0.8564 0.7776 -0.2370 0.025 Uiso 1 1 calc R . .
C30 C 0.76030(14) 0.89771(14) 0.48659(9) 0.0181(3) Uani 1 1 d . . .
H30 H 0.8636 0.8529 0.4793 0.022 Uiso 1 1 calc R . .
C24 C 1.03439(13) 0.62870(13) 0.05904(9) 0.0174(2) Uani 1 1 d . . .
H24 H 0.9722 0.5750 0.0635 0.021 Uiso 1 1 calc R . .
C26 C 0.78356(12) 0.87119(12) 0.31739(9) 0.0138(2) Uani 1 1 d . . .
H26A H 0.8370 0.7806 0.3452 0.017 Uiso 1 1 calc R . .
H26B H 0.8482 0.9076 0.2642 0.017 Uiso 1 1 calc R . .
C5 C 0.30843(15) 0.54155(15) 0.26057(10) 0.0226(3) Uani 1 1 d . . .
H5 H 0.2768 0.4629 0.2652 0.027 Uiso 1 1 calc R . .
C3 C 0.25908(14) 0.78205(15) 0.26942(10) 0.0210(3) Uani 1 1 d . . .
H3 H 0.1933 0.8688 0.2800 0.025 Uiso 1 1 calc R . .
C14 C 0.83556(13) 0.80275(14) -0.09626(9) 0.0185(3) Uani 1 1 d . . .
H14 H 0.9313 0.7963 -0.0996 0.022 Uiso 1 1 calc R . .
C23 C 1.17848(14) 0.56905(15) 0.03744(10) 0.0208(3) Uani 1 1 d . . .
H23 H 1.2145 0.4748 0.0279 0.025 Uiso 1 1 calc R . .
C28 C 0.91968(14) 1.08610(16) 0.34506(12) 0.0253(3) Uani 1 1 d . . .
H28A H 0.9560 1.0384 0.4032 0.038 Uiso 1 1 calc R . .
H28B H 0.9328 1.1782 0.3317 0.038 Uiso 1 1 calc R . .
H28C H 0.9704 1.0342 0.2905 0.038 Uiso 1 1 calc R . .
C32 C 0.71670(17) 0.99832(16) 0.56164(10) 0.0264(3) Uani 1 1 d . . .
H32A H 0.7652 1.0697 0.5395 0.040 Uiso 1 1 calc R . .
H32B H 0.7418 0.9490 0.6228 0.040 Uiso 1 1 calc R . .
H32C H 0.6151 1.0408 0.5707 0.040 Uiso 1 1 calc R . .
C16 C 0.65120(14) 0.80271(15) -0.17481(9) 0.0199(3) Uani 1 1 d . . .
H16 H 0.6209 0.7960 -0.2310 0.024 Uiso 1 1 calc R . .
C22 C 1.26990(14) 0.64820(16) 0.02987(10) 0.0222(3) Uani 1 1 d . . .
H22 H 1.3683 0.6082 0.0135 0.027 Uiso 1 1 calc R . .
C29 C 0.70474(15) 1.17144(14) 0.27097(11) 0.0228(3) Uani 1 1 d . . .
H29A H 0.6047 1.1781 0.2818 0.034 Uiso 1 1 calc R . .
H29B H 0.7547 1.1199 0.2161 0.034 Uiso 1 1 calc R . .
H29C H 0.7171 1.2639 0.2574 0.034 Uiso 1 1 calc R . .
C6 C 0.45122(14) 0.52994(14) 0.23753(10) 0.0194(3) Uani 1 1 d . . .
H6 H 0.5163 0.4433 0.2256 0.023 Uiso 1 1 calc R . .
C4 C 0.21223(14) 0.66773(16) 0.27677(10) 0.0219(3) Uani 1 1 d . . .
H4 H 0.1147 0.6757 0.2928 0.026 Uiso 1 1 calc R . .
C31 C 0.68354(17) 0.78718(16) 0.52245(10) 0.0262(3) Uani 1 1 d . . .
H31A H 0.7106 0.7219 0.4749 0.039 Uiso 1 1 calc R . .
H31B H 0.5821 0.8303 0.5317 0.039 Uiso 1 1 calc R . .
H31C H 0.7087 0.7386 0.5837 0.039 Uiso 1 1 calc R . .


_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 N1 1.7088(10) . ?
P1 C1 1.8365(12) . ?
P1 C7 1.8428(13) . ?
P2 N1 1.7181(11) . ?
P2 C13 1.8306(12) . ?
P2 C19 1.8329(13) . ?
N1 C25 1.4862(14) . ?
N2 C26 1.4743(14) . ?
N2 C30 1.4763(17) . ?
N2 C27 1.4798(16) . ?
C25 C26 1.5272(16) . ?
C1 C2 1.3954(17) . ?
C1 C6 1.4033(17) . ?
C7 C12 1.3979(17) . ?
C7 C8 1.4057(17) . ?
C9 C8 1.385(2) . ?
C9 C10 1.3924(19) . ?
C13 C18 1.4001(17) . ?
C13 C14 1.4028(17) . ?
C27 C29 1.520(2) . ?
C27 C28 1.5306(18) . ?
C12 C11 1.391(2) . ?
C19 C20 1.3954(17) . ?
C19 C24 1.4045(17) . ?
C11 C10 1.3896(18) . ?
C17 C16 1.3867(18) . ?
C17 C18 1.3944(18) . ?
C21 C22 1.383(2) . ?
C21 C20 1.3936(18) . ?
C2 C3 1.3950(17) . ?
C15 C16 1.3867(18) . ?
C15 C14 1.3935(18) . ?
C30 C32 1.5271(17) . ?
C30 C31 1.5300(19) . ?
C24 C23 1.3910(18) . ?
C5 C4 1.386(2) . ?
C5 C6 1.3907(18) . ?
C3 C4 1.384(2) . ?
C23 C22 1.3955(19) . ?

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
N1 P1 C1 104.10(5) . . ?
N1 P1 C7 101.59(5) . . ?
C1 P1 C7 101.75(6) . . ?
N1 P2 C13 104.71(5) . . ?
N1 P2 C19 107.66(6) . . ?
C13 P2 C19 100.69(5) . . ?
C25 N1 P1 122.32(8) . . ?
C25 N1 P2 113.28(8) . . ?
P1 N1 P2 124.29(6) . . ?
C26 N2 C30 111.98(10) . . ?
C26 N2 C27 112.62(10) . . ?
C30 N2 C27 115.07(10) . . ?
N1 C25 C26 113.81(9) . . ?
C2 C1 C6 118.02(11) . . ?
C2 C1 P1 124.37(9) . . ?
C6 C1 P1 117.46(9) . . ?
C12 C7 C8 117.97(12) . . ?
C12 C7 P1 125.98(10) . . ?
C8 C7 P1 115.99(9) . . ?
C8 C9 C10 120.31(12) . . ?
C18 C13 C14 118.12(11) . . ?
C18 C13 P2 120.51(9) . . ?
C14 C13 P2 120.60(9) . . ?
N2 C27 C29 111.19(10) . . ?
N2 C27 C28 114.72(11) . . ?
C29 C27 C28 110.35(12) . . ?
C11 C12 C7 120.98(12) . . ?
C20 C19 C24 118.61(11) . . ?
C20 C19 P2 116.19(10) . . ?
C24 C19 P2 125.08(9) . . ?
C10 C11 C12 120.28(12) . . ?
C16 C17 C18 120.04(12) . . ?
C9 C8 C7 121.00(12) . . ?
C22 C21 C20 119.90(12) . . ?
C21 C20 C19 120.85(12) . . ?
C3 C2 C1 120.71(12) . . ?
C11 C10 C9 119.42(13) . . ?
C17 C18 C13 120.94(11) . . ?
C16 C15 C14 120.16(12) . . ?
N2 C30 C32 112.31(11) . . ?
N2 C30 C31 109.40(11) . . ?
C32 C30 C31 108.65(12) . . ?
C23 C24 C19 120.59(12) . . ?
N2 C26 C25 110.09(9) . . ?
C4 C5 C6 120.11(12) . . ?
C4 C3 C2 120.47(13) . . ?
C15 C14 C13 120.80(12) . . ?
C24 C23 C22 119.77(13) . . ?
C17 C16 C15 119.93(12) . . ?
C21 C22 C23 120.24(12) . . ?
C5 C6 C1 121.04(12) . . ?
C3 C4 C5 119.63(12) . . ?

_diffrn_measured_fraction_theta_max 0.894
_diffrn_reflns_theta_full        28.56
_diffrn_measured_fraction_theta_full 0.894
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 995242'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_c:as28js120c\mono

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H31 N O P2'
_chemical_formula_weight         483.50

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

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                   8.6080(7)
_cell_length_b                   22.5050(8)
_cell_length_c                   13.7650(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.913(2)
_cell_angle_gamma                90.00
_cell_volume                     2551.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    40057
_cell_measurement_theta_min      1.79
_cell_measurement_theta_max      28.86

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Low data completion ratio is due to the limitations of the instrument available
at the Australian Synchrotron operating under rotation data collection with a
fixed detector and affects some high angle data. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'synchrotron BM'
_diffrn_radiation_monochromator  Si<111>
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41516
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         28.86
_reflns_number_total             6283
_reflns_number_gt                6184
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       BLU-ICE
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)' 
;
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

Disorder in one PPh2 unit was observed in difference maps and modelled 
with two complementary populations for the remote 5-carbons of a phyenyl 
ring, with associated hydrogen atoms. The disorder was also apparent 
in the non-centrosymetric space group alternatives.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0166P)²+2.0646P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6283
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.1063
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_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 0.44119(4) 0.166287(15) 0.24344(3) 0.01977(10) Uani 1 1 d . . .
P2 P 0.64195(5) 0.072444(17) 0.20693(3) 0.02512(10) Uani 1 1 d . A .
O1 O 0.60253(15) 0.15250(8) 0.47957(10) 0.0448(4) Uani 1 1 d . . .
N1 N 0.58008(15) 0.11856(5) 0.28475(9) 0.0236(2) Uani 1 1 d . . .
C1 C 0.35592(17) 0.18323(6) 0.34771(11) 0.0226(3) Uani 1 1 d . . .
H1A H 0.3041 0.1460 0.3631 0.027 Uiso 1 1 calc R . .
C2 C 0.49145(19) 0.20009(8) 0.44408(12) 0.0306(3) Uani 1 1 d . . .
H2 H 0.5520 0.2352 0.4290 0.037 Uiso 1 1 calc R . .
C3 C 0.4206(2) 0.21601(9) 0.53014(12) 0.0349(4) Uani 1 1 d . . .
H3A H 0.3716 0.1800 0.5504 0.042 Uiso 1 1 calc R . .
H3B H 0.5094 0.2294 0.5896 0.042 Uiso 1 1 calc R . .
C4 C 0.2928(2) 0.26439(8) 0.50082(14) 0.0358(4) Uani 1 1 d . . .
H4A H 0.2485 0.2724 0.5583 0.043 Uiso 1 1 calc R . .
H4B H 0.3426 0.3015 0.4852 0.043 Uiso 1 1 calc R . .
C5 C 0.1571(2) 0.24521(7) 0.40892(13) 0.0313(3) Uani 1 1 d . . .
H5A H 0.0753 0.2773 0.3893 0.038 Uiso 1 1 calc R . .
H5B H 0.1030 0.2095 0.4260 0.038 Uiso 1 1 calc R . .
C6 C 0.2236(2) 0.23115(7) 0.31975(12) 0.0290(3) Uani 1 1 d . . .
H6A H 0.2691 0.2678 0.2990 0.035 Uiso 1 1 calc R . .
H6B H 0.1337 0.2173 0.2613 0.035 Uiso 1 1 calc R . .
C7 C 0.51688(18) 0.23588(6) 0.20882(10) 0.0215(3) Uani 1 1 d . . .
C8 C 0.68207(19) 0.24804(7) 0.25064(11) 0.0253(3) Uani 1 1 d . . .
H8 H 0.7519 0.2189 0.2907 0.030 Uiso 1 1 calc R . .
C9 C 0.7443(2) 0.30283(7) 0.23359(12) 0.0295(3) Uani 1 1 d . . .
H9 H 0.8567 0.3109 0.2619 0.035 Uiso 1 1 calc R . .
C10 C 0.6433(2) 0.34561(7) 0.17553(12) 0.0302(3) Uani 1 1 d . . .
H10 H 0.6862 0.3833 0.1654 0.036 Uiso 1 1 calc R . .
C11 C 0.4797(2) 0.33357(7) 0.13210(12) 0.0286(3) Uani 1 1 d . . .
H11 H 0.4109 0.3627 0.0913 0.034 Uiso 1 1 calc R . .
C12 C 0.41634(19) 0.27875(6) 0.14834(11) 0.0247(3) Uani 1 1 d . . .
H12 H 0.3044 0.2705 0.1182 0.030 Uiso 1 1 calc R . .
C13 C 0.27781(18) 0.14221(6) 0.13516(11) 0.0227(3) Uani 1 1 d . . .
C14 C 0.2925(2) 0.14864(7) 0.03766(12) 0.0307(3) Uani 1 1 d . . .
H14 H 0.3808 0.1705 0.0273 0.037 Uiso 1 1 calc R . .
C15 C 0.1784(2) 0.12310(8) -0.04450(12) 0.0362(4) Uani 1 1 d . . .
H15 H 0.1895 0.1273 -0.1108 0.043 Uiso 1 1 calc R . .
C16 C 0.0486(2) 0.09161(7) -0.03049(13) 0.0325(3) Uani 1 1 d . . .
H16 H -0.0294 0.0744 -0.0870 0.039 Uiso 1 1 calc R . .
C17 C 0.0330(2) 0.08528(8) 0.06600(13) 0.0344(4) Uani 1 1 d . . .
H17 H -0.0565 0.0639 0.0757 0.041 Uiso 1 1 calc R . .
C18 C 0.1474(2) 0.10992(7) 0.14893(12) 0.0295(3) Uani 1 1 d . . .
H18 H 0.1368 0.1048 0.2152 0.035 Uiso 1 1 calc R . .
C19 C 0.84580(18) 0.05313(6) 0.28663(11) 0.0236(3) Uani 1 1 d . . .
C20 C 0.9233(2) 0.00476(7) 0.25728(13) 0.0286(3) Uani 1 1 d . . .
H20 H 0.8677 -0.0176 0.1990 0.034 Uiso 1 1 calc R . .
C21 C 1.0794(2) -0.01121(8) 0.31150(14) 0.0333(3) Uani 1 1 d . . .
H21 H 1.1305 -0.0441 0.2901 0.040 Uiso 1 1 calc R . .
C22 C 1.1615(2) 0.02077(8) 0.39730(14) 0.0346(4) Uani 1 1 d . . .
H22 H 1.2687 0.0098 0.4349 0.041 Uiso 1 1 calc R . .
C23 C 1.0866(2) 0.06869(8) 0.42781(13) 0.0339(4) Uani 1 1 d . . .
H23 H 1.1424 0.0905 0.4867 0.041 Uiso 1 1 calc R . .
C24 C 0.9292(2) 0.08513(7) 0.37242(12) 0.0287(3) Uani 1 1 d . . .
H24 H 0.8788 0.1183 0.3935 0.034 Uiso 1 1 calc R . .
C25 C 0.54344(19) 0.00204(7) 0.22322(15) 0.0342(4) Uani 1 1 d . . .
C26A C 0.4871(10) -0.0303(3) 0.1250(6) 0.0345(14) Uani 0.50(2) 1 d P A 1
H26A H 0.5038 -0.0156 0.0641 0.041 Uiso 0.50(2) 1 calc PR A 1
C26B C 0.4572(10) -0.0355(3) 0.1542(8) 0.0381(17) Uani 0.50(2) 1 d P A 2
H26B H 0.4405 -0.0252 0.0850 0.046 Uiso 0.50(2) 1 calc PR A 2
C27A C 0.4081(8) -0.0839(3) 0.1290(9) 0.0411(18) Uani 0.50(2) 1 d P A 1
H27A H 0.3650 -0.1065 0.0689 0.049 Uiso 0.50(2) 1 calc PR A 1
C27B C 0.3881(8) -0.0891(3) 0.1734(11) 0.042(2) Uani 0.50(2) 1 d P A 2
H27B H 0.3346 -0.1144 0.1187 0.051 Uiso 0.50(2) 1 calc PR A 2
C28A C 0.3929(7) -0.1038(3) 0.2192(10) 0.0360(18) Uani 0.50(2) 1 d P A 1
H28A H 0.3382 -0.1402 0.2212 0.043 Uiso 0.50(2) 1 calc PR A 1
C28B C 0.3977(7) -0.1051(2) 0.2718(12) 0.042(2) Uani 0.50(2) 1 d P A 2
H28B H 0.3500 -0.1412 0.2848 0.050 Uiso 0.50(2) 1 calc PR A 2
C29A C 0.4548(9) -0.0723(4) 0.3072(9) 0.0359(16) Uani 0.50(2) 1 d P A 1
H29A H 0.4459 -0.0870 0.3701 0.043 Uiso 0.50(2) 1 calc PR A 1
C29B C 0.4768(10) -0.0685(3) 0.3509(10) 0.0376(17) Uani 0.50(2) 1 d P A 2
H29B H 0.4834 -0.0793 0.4188 0.045 Uiso 0.50(2) 1 calc PR A 2
C30A C 0.5489(12) -0.0143(4) 0.3308(8) 0.0223(13) Uani 0.50(2) 1 d P A 2
H30A H 0.6004 0.0115 0.3852 0.027 Uiso 0.50(2) 1 calc PR A 2
C30B C 0.5285(13) -0.0200(5) 0.3027(8) 0.0302(16) Uani 0.50(2) 1 d P A 1
H30B H 0.5718 0.0013 0.3642 0.036 Uiso 0.50(2) 1 calc PR A 1
H1 H 0.619(4) 0.1329(15) 0.426(3) 0.088 Uiso 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 

 Hydrogen bonds with  H..A < r(A) + 2.000 Angstroms  and  <DHA > 110 deg.

 D-H           d(D-H)   d(H..A)   <DHA    d(D..A)   A

 O1-H1          0.910    1.897   153.32    2.741    N1 

;

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 N1 1.5846(13) . ?
P1 C13 1.8092(15) . ?
P1 C7 1.8126(14) . ?
P1 C1 1.8322(15) . ?
P2 N1 1.6853(13) . ?
P2 C19 1.8307(16) . ?
P2 C25 1.8413(18) . ?
O1 C2 1.424(2) . ?
O1 H1 0.91(4) . ?
C1 C6 1.534(2) . ?
C1 C2 1.538(2) . ?
C1 H1A 1.0000 . ?
C2 C3 1.524(2) . ?
C2 H2 1.0000 . ?
C3 C4 1.517(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.514(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.531(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.397(2) . ?
C7 C12 1.398(2) . ?
C8 C9 1.391(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.392(2) . ?
C13 C18 1.396(2) . ?
C14 C15 1.389(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(2) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.391(2) . ?
C19 C20 1.396(2) . ?
C20 C21 1.381(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.383(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.398(2) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30B 1.242(11) . ?
C25 C26B 1.326(8) . ?
C25 C26A 1.487(7) . ?
C25 C30A 1.513(10) . ?
C26A C27A 1.393(9) . ?
C26A H26A 0.9500 . ?
C26B C27B 1.404(9) . ?
C26B H26B 0.9500 . ?
C27A C28A 1.362(8) . ?
C27A H27A 0.9500 . ?
C27B C28B 1.380(9) . ?
C27B H27B 0.9500 . ?
C28A C29A 1.371(9) . ?
C28A H28A 0.9500 . ?
C28B C29B 1.377(9) . ?
C28B H28B 0.9500 . ?
C29A C30B 1.346(13) . ?
C29A H29A 0.9500 . ?
C29B C30A 1.432(11) . ?
C29B H29B 0.9500 . ?
C30A H30A 0.9500 . ?
C30B H30B 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C13 114.66(7) . . ?
N1 P1 C7 112.87(7) . . ?
C13 P1 C7 107.15(7) . . ?
N1 P1 C1 107.00(7) . . ?
C13 P1 C1 108.37(7) . . ?
C7 P1 C1 106.42(6) . . ?
N1 P2 C19 100.98(6) . . ?
N1 P2 C25 102.16(8) . . ?
C19 P2 C25 96.77(7) . . ?
C2 O1 H1 109(2) . . ?
P1 N1 P2 122.30(8) . . ?
C6 C1 C2 111.38(13) . . ?
C6 C1 P1 112.78(10) . . ?
C2 C1 P1 110.54(10) . . ?
C6 C1 H1A 107.3 . . ?
C2 C1 H1A 107.3 . . ?
P1 C1 H1A 107.3 . . ?
O1 C2 C3 106.89(14) . . ?
O1 C2 C1 112.05(13) . . ?
C3 C2 C1 110.73(13) . . ?
O1 C2 H2 109.0 . . ?
C3 C2 H2 109.0 . . ?
C1 C2 H2 109.0 . . ?
C4 C3 C2 112.64(15) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 C3 109.98(14) . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C4 C5 C6 110.55(14) . . ?
C4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C5 C6 C1 111.58(12) . . ?
C5 C6 H6A 109.3 . . ?
C1 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
C1 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C12 119.33(13) . . ?
C8 C7 P1 117.49(11) . . ?
C12 C7 P1 123.05(11) . . ?
C9 C8 C7 119.98(14) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.39(15) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 120.06(14) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 C12 119.98(15) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C7 120.22(14) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
C14 C13 C18 119.17(14) . . ?
C14 C13 P1 119.76(12) . . ?
C18 C13 P1 120.48(11) . . ?
C15 C14 C13 120.06(15) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 120.50(15) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 119.70(15) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.40(15) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C13 120.15(15) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.9 . . ?
C24 C19 C20 118.51(14) . . ?
C24 C19 P2 123.61(12) . . ?
C20 C19 P2 117.84(12) . . ?
C21 C20 C19 121.20(15) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C20 C21 C22 119.97(15) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 119.71(16) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.29(16) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C19 C24 C23 120.33(15) . . ?
C19 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C30B C25 C26B 101.3(9) . . ?
C30B C25 C26A 121.0(7) . . ?
C26B C25 C26A 21.5(3) . . ?
C30B C25 C30A 12.1(6) . . ?
C26B C25 C30A 113.4(8) . . ?
C26A C25 C30A 132.8(6) . . ?
C30B C25 P2 128.4(5) . . ?
C26B C25 P2 130.0(5) . . ?
C26A C25 P2 110.5(4) . . ?
C30A C25 P2 116.4(3) . . ?
C27A C26A C25 115.0(5) . . ?
C27A C26A H26A 122.5 . . ?
C25 C26A H26A 122.5 . . ?
C25 C26B C27B 126.3(7) . . ?
C25 C26B H26B 116.8 . . ?
C27B C26B H26B 116.8 . . ?
C28A C27A C26A 119.9(6) . . ?
C28A C27A H27A 120.1 . . ?
C26A C27A H27A 120.1 . . ?
C28B C27B C26B 120.1(6) . . ?
C28B C27B H27B 120.0 . . ?
C26B C27B H27B 120.0 . . ?
C27A C28A C29A 121.3(6) . . ?
C27A C28A H28A 119.3 . . ?
C29A C28A H28A 119.3 . . ?
C29B C28B C27B 119.7(5) . . ?
C29B C28B H28B 120.2 . . ?
C27B C28B H28B 120.2 . . ?
C30B C29A C28A 118.6(8) . . ?
C30B C29A H29A 120.7 . . ?
C28A C29A H29A 120.7 . . ?
C28B C29B C30A 119.9(8) . . ?
C28B C29B H29B 120.0 . . ?
C30A C29B H29B 120.0 . . ?
C29B C30A C25 120.3(11) . . ?
C29B C30A H30A 119.9 . . ?
C25 C30A H30A 119.9 . . ?
C25 C30B C29A 124.1(11) . . ?
C25 C30B H30B 117.9 . . ?
C29A C30B H30B 117.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 P1 N1 P2 36.53(11) . . . . ?
C7 P1 N1 P2 -86.55(10) . . . . ?
C1 P1 N1 P2 156.72(8) . . . . ?
C19 P2 N1 P1 157.35(9) . . . . ?
C25 P2 N1 P1 -103.17(10) . . . . ?
N1 P1 C1 C6 177.64(11) . . . . ?
C13 P1 C1 C6 -58.23(12) . . . . ?
C7 P1 C1 C6 56.72(12) . . . . ?
N1 P1 C1 C2 52.22(12) . . . . ?
C13 P1 C1 C2 176.35(11) . . . . ?
C7 P1 C1 C2 -68.70(12) . . . . ?
C6 C1 C2 O1 171.34(13) . . . . ?
P1 C1 C2 O1 -62.45(15) . . . . ?
C6 C1 C2 C3 52.11(18) . . . . ?
P1 C1 C2 C3 178.32(12) . . . . ?
O1 C2 C3 C4 -177.05(14) . . . . ?
C1 C2 C3 C4 -54.8(2) . . . . ?
C2 C3 C4 C5 57.83(19) . . . . ?
C3 C4 C5 C6 -57.99(18) . . . . ?
C4 C5 C6 C1 56.96(18) . . . . ?
C2 C1 C6 C5 -53.92(18) . . . . ?
P1 C1 C6 C5 -178.88(11) . . . . ?
N1 P1 C7 C8 -20.48(13) . . . . ?
C13 P1 C7 C8 -147.64(11) . . . . ?
C1 P1 C7 C8 96.59(12) . . . . ?
N1 P1 C7 C12 163.75(12) . . . . ?
C13 P1 C7 C12 36.59(14) . . . . ?
C1 P1 C7 C12 -79.18(13) . . . . ?
C12 C7 C8 C9 1.3(2) . . . . ?
P1 C7 C8 C9 -174.64(12) . . . . ?
C7 C8 C9 C10 0.2(2) . . . . ?
C8 C9 C10 C11 -1.4(2) . . . . ?
C9 C10 C11 C12 1.1(2) . . . . ?
C10 C11 C12 C7 0.4(2) . . . . ?
C8 C7 C12 C11 -1.6(2) . . . . ?
P1 C7 C12 C11 174.11(12) . . . . ?
N1 P1 C13 C14 -85.53(14) . . . . ?
C7 P1 C13 C14 40.57(14) . . . . ?
C1 P1 C13 C14 155.04(13) . . . . ?
N1 P1 C13 C18 85.57(14) . . . . ?
C7 P1 C13 C18 -148.33(13) . . . . ?
C1 P1 C13 C18 -33.86(15) . . . . ?
C18 C13 C14 C15 0.0(2) . . . . ?
P1 C13 C14 C15 171.22(14) . . . . ?
C13 C14 C15 C16 0.6(3) . . . . ?
C14 C15 C16 C17 -0.3(3) . . . . ?
C15 C16 C17 C18 -0.5(3) . . . . ?
C16 C17 C18 C13 1.1(3) . . . . ?
C14 C13 C18 C17 -0.8(2) . . . . ?
P1 C13 C18 C17 -171.98(13) . . . . ?
N1 P2 C19 C24 -16.61(14) . . . . ?
C25 P2 C19 C24 -120.44(14) . . . . ?
N1 P2 C19 C20 165.63(12) . . . . ?
C25 P2 C19 C20 61.80(13) . . . . ?
C24 C19 C20 C21 -0.2(2) . . . . ?
P2 C19 C20 C21 177.68(13) . . . . ?
C19 C20 C21 C22 0.5(3) . . . . ?
C20 C21 C22 C23 -0.3(3) . . . . ?
C21 C22 C23 C24 -0.3(3) . . . . ?
C20 C19 C24 C23 -0.3(2) . . . . ?
P2 C19 C24 C23 -178.08(13) . . . . ?
C22 C23 C24 C19 0.6(3) . . . . ?
N1 P2 C25 C30B -41.1(7) . . . . ?
C19 P2 C25 C30B 61.7(7) . . . . ?
N1 P2 C25 C26B 131.7(5) . . . . ?
C19 P2 C25 C26B -125.5(5) . . . . ?
N1 P2 C25 C26A 142.5(3) . . . . ?
C19 P2 C25 C26A -114.7(3) . . . . ?
N1 P2 C25 C30A -43.0(4) . . . . ?
C19 P2 C25 C30A 59.8(4) . . . . ?
C30B C25 C26A C27A 4.3(10) . . . . ?
C26B C25 C26A C27A -21.8(12) . . . . ?
C30A C25 C26A C27A 7.8(10) . . . . ?
P2 C25 C26A C27A -178.9(5) . . . . ?
C30B C25 C26B C27B -6.9(9) . . . . ?
C26A C25 C26B C27B 150(2) . . . . ?
C30A C25 C26B C27B -6.3(9) . . . . ?
P2 C25 C26B C27B 178.9(5) . . . . ?
C25 C26A C27A C28A -2.3(9) . . . . ?
C25 C26B C27B C28B 4.4(11) . . . . ?
C26A C27A C28A C29A -0.4(10) . . . . ?
C26B C27B C28B C29B -0.6(10) . . . . ?
C27A C28A C29A C30B 1.6(11) . . . . ?
C27B C28B C29B C30A -0.2(10) . . . . ?
C28B C29B C30A C25 -2.0(12) . . . . ?
C30B C25 C30A C29B 8(4) . . . . ?
C26B C25 C30A C29B 5.0(10) . . . . ?
C26A C25 C30A C29B -6.4(12) . . . . ?
P2 C25 C30A C29B -179.4(6) . . . . ?
C26B C25 C30B C29A 6.0(12) . . . . ?
C26A C25 C30B C29A -3.5(14) . . . . ?
C30A C25 C30B C29A -171(5) . . . . ?
P2 C25 C30B C29A -179.6(6) . . . . ?
C28A C29A C30B C25 0.5(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.939
_diffrn_reflns_theta_full        28.86
_diffrn_measured_fraction_theta_full 0.939
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.046
_database_code_depnum_ccdc_archive 'CCDC 995243'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_d:\gard2m~1\as30js32\temp

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33.50 H34 Cl5 N O P2 Si Ti'
_chemical_formula_weight         781.80

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'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

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

_cell_length_a                   11.5300(8)
_cell_length_b                   15.3370(7)
_cell_length_c                   20.8500(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.737(3)
_cell_angle_gamma                90.00
_cell_volume                     3581.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    60969
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      30.86

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1604
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Low data completion ratio is due to the limitations of the instrument available
at the Australian Synchrotron operating under rotation data collection with a
fixed detector and affects some high angle data. 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Synchrotron ID'
_diffrn_radiation_monochromator  Si<111>
_diffrn_measurement_device_type  '3-ID1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_detector_area_resol_mean 'ADSC Q315'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            77400
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         30.86
_reflns_number_total             20509
_reflns_number_gt                18238
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       BLU-ICE
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)' 
;
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

Refinement in P21/m resulted in R1 >11% and a disordered DCM molecule 
that was not present in the P21 refinement (R1 <5%). For these reasons 
the non-centrosymmetric model was preferred.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0591P)²+4.6124P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.53(3)
_refine_ls_number_reflns         20509
_refine_ls_number_parameters     808
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1448
_refine_ls_wR_factor_gt          0.1102
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.56418(4) 0.39341(5) 0.33529(2) 0.01670(10) Uani 1 1 d . . .
Ti2 Ti 1.48785(4) 0.38913(6) 0.73600(2) 0.02087(11) Uani 1 1 d . . .
Cl1 Cl 0.48981(5) 0.39246(8) 0.42730(3) 0.02044(13) Uani 1 1 d . . .
Cl2 Cl 0.68090(6) 0.39294(8) 0.25973(3) 0.02232(13) Uani 1 1 d . . .
Cl3 Cl 0.46529(8) 0.27199(7) 0.29188(5) 0.02429(18) Uani 1 1 d . . .
Cl4 Cl 0.47477(8) 0.52050(7) 0.29526(5) 0.02361(18) Uani 1 1 d . . .
Cl5 Cl 1.33587(6) 0.39389(8) 0.78981(3) 0.02660(15) Uani 1 1 d . . .
Cl6 Cl 1.67081(6) 0.38303(8) 0.71102(4) 0.02582(16) Uani 1 1 d . . .
Cl7 Cl 1.42172(9) 0.26686(8) 0.68035(5) 0.0306(2) Uani 1 1 d . . .
Cl8 Cl 1.43455(10) 0.51334(8) 0.68070(6) 0.0336(2) Uani 1 1 d . . .
Cl9 Cl 0.3904(2) 0.40872(16) 0.06231(7) 0.0883(8) Uani 1 1 d . . .
Cl10 Cl 0.24007(13) 0.35719(17) 0.14678(12) 0.1046(10) Uani 1 1 d . . .
P1 P 0.73678(8) 0.29958(6) 0.40864(4) 0.01612(17) Uani 1 1 d . . .
P2 P 0.74209(7) 0.47988(6) 0.41139(4) 0.01616(17) Uani 1 1 d . . .
P3 P 1.58920(8) 0.29923(7) 0.84219(5) 0.01856(18) Uani 1 1 d . . .
P4 P 1.60017(8) 0.47863(7) 0.84046(5) 0.01899(18) Uani 1 1 d . . .
Si1 Si 1.07846(7) 0.38749(13) 0.32447(4) 0.0332(2) Uani 1 1 d . . .
Si2 Si 2.01234(8) 0.37235(7) 0.86665(5) 0.0258(2) Uani 1 1 d . . .
O1 O 0.99641(17) 0.3883(3) 0.38078(9) 0.0264(5) Uani 1 1 d . . .
O7 O 1.87823(19) 0.3760(2) 0.88638(11) 0.0236(6) Uani 1 1 d . . .
N1 N 0.81725(18) 0.3877(2) 0.44500(10) 0.0164(4) Uani 1 1 d . . .
N2 N 1.64059(19) 0.3886(3) 0.88990(10) 0.0179(4) Uani 1 1 d . . .
C1 C 1.0304(2) 0.3863(3) 0.44736(13) 0.0207(6) Uani 1 1 d . . .
C2 C 0.9398(2) 0.3857(3) 0.48205(13) 0.0183(5) Uani 1 1 d . . .
C3 C 0.9685(3) 0.3837(3) 0.55077(13) 0.0224(6) Uani 1 1 d . . .
H3 H 0.9068 0.3830 0.5739 0.027 Uiso 1 1 calc R . .
C4 C 1.0874(3) 0.3826(3) 0.58559(15) 0.0280(7) Uani 1 1 d . . .
H4 H 1.1072 0.3817 0.6325 0.034 Uiso 1 1 calc R . .
C5 C 1.1771(3) 0.3827(3) 0.55109(16) 0.0261(7) Uani 1 1 d . . .
H5 H 1.2584 0.3819 0.5747 0.031 Uiso 1 1 calc R . .
C6 C 1.1491(2) 0.3839(3) 0.48295(15) 0.0249(7) Uani 1 1 d . . .
H6 H 1.2112 0.3831 0.4601 0.030 Uiso 1 1 calc R . .
C7 C 0.7041(3) 0.2305(2) 0.47290(18) 0.0169(6) Uani 1 1 d . . .
C8 C 0.6870(3) 0.1419(3) 0.4604(2) 0.0234(8) Uani 1 1 d . . .
H8 H 0.7014 0.1179 0.4210 0.028 Uiso 1 1 calc R . .
C9 C 0.6488(4) 0.0876(3) 0.5052(2) 0.0292(9) Uani 1 1 d . . .
H9 H 0.6364 0.0272 0.4960 0.035 Uiso 1 1 calc R . .
C10 C 0.6289(4) 0.1225(3) 0.5637(2) 0.0292(9) Uani 1 1 d . . .
H10 H 0.6022 0.0860 0.5942 0.035 Uiso 1 1 calc R . .
C11 C 0.6484(4) 0.2104(3) 0.5769(2) 0.0257(8) Uani 1 1 d . . .
H11 H 0.6372 0.2342 0.6171 0.031 Uiso 1 1 calc R . .
C12 C 0.6845(3) 0.2639(3) 0.5315(2) 0.0229(7) Uani 1 1 d . . .
H12 H 0.6959 0.3244 0.5406 0.027 Uiso 1 1 calc R . .
C13 C 0.8274(3) 0.2246(3) 0.37362(19) 0.0188(7) Uani 1 1 d . . .
C14 C 0.7818(4) 0.1912(3) 0.3110(2) 0.0266(8) Uani 1 1 d . . .
H14 H 0.7109 0.2151 0.2839 0.032 Uiso 1 1 calc R . .
C15 C 0.8402(4) 0.1226(3) 0.2877(2) 0.0316(9) Uani 1 1 d . . .
H15 H 0.8084 0.0993 0.2450 0.038 Uiso 1 1 calc R . .
C16 C 0.9438(4) 0.0888(3) 0.3269(2) 0.0338(10) Uani 1 1 d . . .
H16 H 0.9836 0.0423 0.3109 0.041 Uiso 1 1 calc R . .
C17 C 0.9902(4) 0.1222(3) 0.3893(2) 0.0315(9) Uani 1 1 d . . .
H17 H 1.0621 0.0989 0.4157 0.038 Uiso 1 1 calc R . .
C18 C 0.9324(3) 0.1897(3) 0.4135(2) 0.0233(7) Uani 1 1 d . . .
H18 H 0.9638 0.2120 0.4567 0.028 Uiso 1 1 calc R . .
C19 C 0.7104(3) 0.5467(2) 0.47697(19) 0.0178(7) Uani 1 1 d . . .
C20 C 0.6953(4) 0.5120(3) 0.5367(2) 0.0229(7) Uani 1 1 d . . .
H20 H 0.7112 0.4521 0.5466 0.027 Uiso 1 1 calc R . .
C21 C 0.6570(4) 0.5655(3) 0.5813(2) 0.0274(9) Uani 1 1 d . . .
H21 H 0.6474 0.5419 0.6218 0.033 Uiso 1 1 calc R . .
C22 C 0.6330(4) 0.6520(3) 0.5677(2) 0.0307(9) Uani 1 1 d . . .
H22 H 0.6049 0.6877 0.5981 0.037 Uiso 1 1 calc R . .
C23 C 0.6499(4) 0.6872(3) 0.5091(3) 0.0312(9) Uani 1 1 d . . .
H23 H 0.6345 0.7473 0.4999 0.037 Uiso 1 1 calc R . .
C24 C 0.6890(4) 0.6355(3) 0.4644(2) 0.0246(8) Uani 1 1 d . . .
H24 H 0.7014 0.6604 0.4248 0.030 Uiso 1 1 calc R . .
C25 C 0.8387(3) 0.5537(3) 0.37949(19) 0.0196(7) Uani 1 1 d . . .
C26 C 0.7995(4) 0.5886(3) 0.3163(2) 0.0262(8) Uani 1 1 d . . .
H26 H 0.7270 0.5687 0.2882 0.031 Uiso 1 1 calc R . .
C27 C 0.8668(4) 0.6526(3) 0.2943(2) 0.0308(9) Uani 1 1 d . . .
H27 H 0.8402 0.6768 0.2513 0.037 Uiso 1 1 calc R . .
C28 C 0.9730(4) 0.6808(3) 0.3357(2) 0.0324(9) Uani 1 1 d . . .
H28 H 1.0197 0.7236 0.3205 0.039 Uiso 1 1 calc R . .
C29 C 1.0115(4) 0.6476(3) 0.3985(2) 0.0271(8) Uani 1 1 d . . .
H29 H 1.0839 0.6679 0.4264 0.033 Uiso 1 1 calc R . .
C30 C 0.9445(3) 0.5844(3) 0.4211(2) 0.0225(7) Uani 1 1 d . . .
H30 H 0.9704 0.5621 0.4646 0.027 Uiso 1 1 calc R . .
C31 C 0.9691(4) 0.3987(11) 0.24426(19) 0.112(4) Uani 1 1 d . . .
H31A H 0.9209 0.3455 0.2351 0.168 Uiso 1 1 calc R . .
H31B H 1.0115 0.4078 0.2093 0.168 Uiso 1 1 calc R . .
H31C H 0.9169 0.4486 0.2459 0.168 Uiso 1 1 calc R . .
C32 C 1.1641(7) 0.2859(4) 0.3300(4) 0.0605(19) Uani 1 1 d . . .
H32A H 1.2181 0.2812 0.3739 0.091 Uiso 1 1 calc R . .
H32B H 1.2107 0.2859 0.2963 0.091 Uiso 1 1 calc R . .
H32C H 1.1091 0.2361 0.3226 0.091 Uiso 1 1 calc R . .
C33 C 1.1826(5) 0.4819(4) 0.3369(3) 0.0436(12) Uani 1 1 d . . .
H33A H 1.1394 0.5349 0.3436 0.065 Uiso 1 1 calc R . .
H33B H 1.2152 0.4890 0.2979 0.065 Uiso 1 1 calc R . .
H33C H 1.2479 0.4715 0.3758 0.065 Uiso 1 1 calc R . .
C34 C 1.8541(3) 0.3796(3) 0.94620(15) 0.0209(7) Uani 1 1 d . . .
C35 C 1.7337(2) 0.3871(3) 0.94992(13) 0.0195(5) Uani 1 1 d . . .
C36 C 1.7051(3) 0.3937(3) 1.01087(13) 0.0221(5) Uani 1 1 d . . .
H36 H 1.6240 0.3997 1.0128 0.027 Uiso 1 1 calc R . .
C37 C 1.7940(3) 0.3916(4) 1.06897(13) 0.0264(6) Uani 1 1 d . . .
H37 H 1.7741 0.3967 1.1105 0.032 Uiso 1 1 calc R . .
C38 C 1.9116(3) 0.3820(4) 1.06560(16) 0.0302(8) Uani 1 1 d . . .
H38 H 1.9727 0.3795 1.1052 0.036 Uiso 1 1 calc R . .
C39 C 1.9416(3) 0.3759(3) 1.00550(17) 0.0286(9) Uani 1 1 d . . .
H39 H 2.0230 0.3691 1.0044 0.034 Uiso 1 1 calc R . .
C40 C 1.4893(3) 0.2349(3) 0.8794(2) 0.0219(7) Uani 1 1 d . . .
C41 C 1.4481(4) 0.1581(3) 0.8455(2) 0.0314(9) Uani 1 1 d . . .
H41 H 1.4710 0.1441 0.8059 0.038 Uiso 1 1 calc R . .
C42 C 1.3737(4) 0.1021(3) 0.8699(2) 0.0314(9) Uani 1 1 d . . .
H42 H 1.3458 0.0498 0.8470 0.038 Uiso 1 1 calc R . .
C43 C 1.3406(4) 0.1228(3) 0.9273(2) 0.0277(8) Uani 1 1 d . . .
H43 H 1.2895 0.0848 0.9439 0.033 Uiso 1 1 calc R . .
C44 C 1.3817(3) 0.1992(3) 0.9613(2) 0.0272(8) Uani 1 1 d . . .
H44 H 1.3598 0.2128 1.0013 0.033 Uiso 1 1 calc R . .
C45 C 1.4553(3) 0.2557(3) 0.93652(19) 0.0233(7) Uani 1 1 d . . .
H45 H 1.4819 0.3085 0.9590 0.028 Uiso 1 1 calc R . .
C46 C 1.7092(3) 0.2198(3) 0.85085(19) 0.0199(7) Uani 1 1 d . . .
C47 C 1.7534(3) 0.1803(3) 0.9123(2) 0.0273(8) Uani 1 1 d . . .
H47 H 1.7246 0.1983 0.9493 0.033 Uiso 1 1 calc R . .
C48 C 1.8387(4) 0.1154(3) 0.9196(3) 0.0386(10) Uani 1 1 d . . .
H48 H 1.8686 0.0891 0.9615 0.046 Uiso 1 1 calc R . .
C49 C 1.8808(5) 0.0883(4) 0.8653(3) 0.0435(11) Uani 1 1 d . . .
H49 H 1.9392 0.0435 0.8701 0.052 Uiso 1 1 calc R . .
C50 C 1.8370(5) 0.1271(3) 0.8046(3) 0.0407(11) Uani 1 1 d . . .
H50 H 1.8663 0.1092 0.7677 0.049 Uiso 1 1 calc R . .
C51 C 1.7508(4) 0.1920(3) 0.7968(2) 0.0303(9) Uani 1 1 d . . .
H51 H 1.7201 0.2174 0.7546 0.036 Uiso 1 1 calc R . .
C52 C 1.5065(3) 0.5506(3) 0.87560(19) 0.0214(7) Uani 1 1 d . . .
C53 C 1.4449(3) 0.5256(3) 0.9226(2) 0.0247(8) Uani 1 1 d . . .
H53 H 1.4545 0.4684 0.9406 0.030 Uiso 1 1 calc R . .
C54 C 1.3694(4) 0.5845(3) 0.9431(2) 0.0281(8) Uani 1 1 d . . .
H54 H 1.3304 0.5682 0.9767 0.034 Uiso 1 1 calc R . .
C55 C 1.3505(4) 0.6666(3) 0.9152(2) 0.0316(9) Uani 1 1 d . . .
H55 H 1.2974 0.7060 0.9287 0.038 Uiso 1 1 calc R . .
C56 C 1.4097(4) 0.6916(3) 0.8669(2) 0.0301(9) Uani 1 1 d . . .
H56 H 1.3962 0.7476 0.8472 0.036 Uiso 1 1 calc R . .
C57 C 1.4886(4) 0.6337(3) 0.8479(2) 0.0275(8) Uani 1 1 d . . .
H57 H 1.5304 0.6511 0.8159 0.033 Uiso 1 1 calc R . .
C58 C 1.7317(3) 0.5482(3) 0.8482(2) 0.0212(7) Uani 1 1 d . . .
C59 C 1.7749(4) 0.5701(3) 0.7937(2) 0.0290(8) Uani 1 1 d . . .
H59 H 1.7390 0.5469 0.7514 0.035 Uiso 1 1 calc R . .
C60 C 1.8721(5) 0.6269(3) 0.8017(3) 0.0411(11) Uani 1 1 d . . .
H60 H 1.9024 0.6416 0.7645 0.049 Uiso 1 1 calc R . .
C61 C 1.9246(4) 0.6618(3) 0.8621(3) 0.0436(11) Uani 1 1 d . . .
H61 H 1.9919 0.6991 0.8668 0.052 Uiso 1 1 calc R . .
C62 C 1.8791(4) 0.6425(3) 0.9166(3) 0.0368(10) Uani 1 1 d . . .
H62 H 1.9138 0.6677 0.9584 0.044 Uiso 1 1 calc R . .
C63 C 1.7826(4) 0.5860(3) 0.9095(2) 0.0292(8) Uani 1 1 d . . .
H63 H 1.7509 0.5731 0.9465 0.035 Uiso 1 1 calc R . .
C64 C 1.9763(3) 0.3774(4) 0.77559(18) 0.0329(9) Uani 1 1 d . . .
H64A H 1.9202 0.3307 0.7574 0.049 Uiso 1 1 calc R . .
H64B H 2.0496 0.3704 0.7601 0.049 Uiso 1 1 calc R . .
H64C H 1.9400 0.4340 0.7609 0.049 Uiso 1 1 calc R . .
C65 C 2.0915(4) 0.2692(4) 0.8967(3) 0.0452(12) Uani 1 1 d . . .
H65A H 2.1178 0.2706 0.9449 0.068 Uiso 1 1 calc R . .
H65B H 2.1611 0.2628 0.8777 0.068 Uiso 1 1 calc R . .
H65C H 2.0374 0.2197 0.8831 0.068 Uiso 1 1 calc R . .
C66 C 2.1065(4) 0.4658(4) 0.9026(3) 0.0416(11) Uani 1 1 d . . .
H66A H 2.0599 0.5197 0.8934 0.062 Uiso 1 1 calc R . .
H66B H 2.1757 0.4694 0.8831 0.062 Uiso 1 1 calc R . .
H66C H 2.1338 0.4579 0.9505 0.062 Uiso 1 1 calc R . .
C67 C 0.3633(4) 0.4172(3) 0.14024(19) 0.0381(11) Uani 1 1 d . . .
H67A H 0.4341 0.3963 0.1735 0.046 Uiso 1 1 calc R . .
H67B H 0.3505 0.4792 0.1498 0.046 Uiso 1 1 calc R . .


_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
Ti1 Cl3 2.2577(12) . ?
Ti1 Cl4 2.2694(12) . ?
Ti1 Cl1 2.2796(8) . ?
Ti1 Cl2 2.3022(8) . ?
Ti1 P1 2.6314(11) . ?
Ti1 P2 2.6340(11) . ?
Ti2 Cl8 2.2360(14) . ?
Ti2 Cl7 2.2414(14) . ?
Ti2 Cl6 2.2917(9) . ?
Ti2 Cl5 2.2953(9) . ?
Ti2 P3 2.6344(12) . ?
Ti2 P4 2.6393(12) . ?
Cl9 C67 1.730(4) . ?
Cl10 C67 1.725(5) . ?
P1 N1 1.711(4) . ?
P1 C7 1.816(4) . ?
P1 C13 1.820(4) . ?
P2 N1 1.718(3) . ?
P2 C19 1.814(4) . ?
P2 C25 1.822(4) . ?
P3 N2 1.715(4) . ?
P3 C46 1.820(4) . ?
P3 C40 1.824(4) . ?
P4 N2 1.720(4) . ?
P4 C52 1.816(4) . ?
P4 C58 1.830(4) . ?
Si1 O1 1.674(2) . ?
Si1 C32 1.834(7) . ?
Si1 C31 1.848(4) . ?
Si1 C33 1.859(6) . ?
Si2 O7 1.693(2) . ?
Si2 C64 1.846(4) . ?
Si2 C66 1.847(5) . ?
Si2 C65 1.859(5) . ?
O1 C1 1.350(3) . ?
O7 C34 1.342(4) . ?
N1 C2 1.440(3) . ?
N2 C35 1.442(3) . ?
C1 C6 1.393(4) . ?
C1 C2 1.405(4) . ?
C2 C3 1.392(4) . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.390(6) . ?
C7 C12 1.391(5) . ?
C8 C9 1.398(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.400(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.384(6) . ?
C13 C18 1.402(5) . ?
C14 C15 1.397(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.379(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.389(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.398(6) . ?
C19 C20 1.402(5) . ?
C20 C21 1.389(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.370(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.390(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.394(6) . ?
C25 C30 1.399(5) . ?
C26 C27 1.395(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.389(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.376(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.389(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C39 1.399(4) . ?
C34 C35 1.413(4) . ?
C35 C36 1.390(4) . ?
C36 C37 1.389(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.383(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.380(5) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C45 1.378(6) . ?
C40 C41 1.396(6) . ?
C41 C42 1.393(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.378(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.393(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.395(6) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C51 1.392(6) . ?
C46 C47 1.399(6) . ?
C47 C48 1.383(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.396(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.382(8) . ?
C49 H49 0.9500 . ?
C50 C51 1.389(7) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.394(6) . ?
C52 C57 1.394(6) . ?
C53 C54 1.391(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.384(7) . ?
C54 H54 0.9500 . ?
C55 C56 1.396(7) . ?
C55 H55 0.9500 . ?
C56 C57 1.394(6) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 C59 1.388(5) . ?
C58 C63 1.398(6) . ?
C59 C60 1.397(7) . ?
C59 H59 0.9500 . ?
C60 C61 1.369(8) . ?
C60 H60 0.9500 . ?
C61 C62 1.392(7) . ?
C61 H61 0.9500 . ?
C62 C63 1.390(6) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?

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
Cl3 Ti1 Cl4 114.77(4) . . ?
Cl3 Ti1 Cl1 94.42(4) . . ?
Cl4 Ti1 Cl1 94.95(4) . . ?
Cl3 Ti1 Cl2 92.56(4) . . ?
Cl4 Ti1 Cl2 92.25(4) . . ?
Cl1 Ti1 Cl2 166.82(3) . . ?
Cl3 Ti1 P1 91.27(4) . . ?
Cl4 Ti1 P1 153.93(4) . . ?
Cl1 Ti1 P1 83.75(3) . . ?
Cl2 Ti1 P1 84.93(3) . . ?
Cl3 Ti1 P2 154.65(4) . . ?
Cl4 Ti1 P2 90.57(4) . . ?
Cl1 Ti1 P2 83.75(3) . . ?
Cl2 Ti1 P2 85.16(3) . . ?
P1 Ti1 P2 63.38(3) . . ?
Cl8 Ti2 Cl7 115.33(4) . . ?
Cl8 Ti2 Cl6 94.17(5) . . ?
Cl7 Ti2 Cl6 93.82(5) . . ?
Cl8 Ti2 Cl5 94.40(5) . . ?
Cl7 Ti2 Cl5 94.26(5) . . ?
Cl6 Ti2 Cl5 164.40(3) . . ?
Cl8 Ti2 P3 153.13(5) . . ?
Cl7 Ti2 P3 91.47(5) . . ?
Cl6 Ti2 P3 85.47(4) . . ?
Cl5 Ti2 P3 81.00(4) . . ?
Cl8 Ti2 P4 90.19(5) . . ?
Cl7 Ti2 P4 154.46(5) . . ?
Cl6 Ti2 P4 84.89(3) . . ?
Cl5 Ti2 P4 82.07(4) . . ?
P3 Ti2 P4 62.99(3) . . ?
N1 P1 C7 108.63(15) . . ?
N1 P1 C13 111.98(15) . . ?
C7 P1 C13 99.62(18) . . ?
N1 P1 Ti1 94.66(10) . . ?
C7 P1 Ti1 119.12(11) . . ?
C13 P1 Ti1 122.67(13) . . ?
N1 P2 C19 109.26(15) . . ?
N1 P2 C25 111.56(15) . . ?
C19 P2 C25 100.03(18) . . ?
N1 P2 Ti1 94.39(11) . . ?
C19 P2 Ti1 118.09(11) . . ?
C25 P2 Ti1 123.33(13) . . ?
N2 P3 C46 109.13(15) . . ?
N2 P3 C40 110.62(16) . . ?
C46 P3 C40 97.91(18) . . ?
N2 P3 Ti2 95.30(11) . . ?
C46 P3 Ti2 127.50(13) . . ?
C40 P3 Ti2 116.20(13) . . ?
N2 P4 C52 110.40(16) . . ?
N2 P4 C58 108.30(16) . . ?
C52 P4 C58 99.76(18) . . ?
N2 P4 Ti2 95.00(11) . . ?
C52 P4 Ti2 115.27(13) . . ?
C58 P4 Ti2 127.63(13) . . ?
O1 Si1 C32 110.4(3) . . ?
O1 Si1 C31 104.85(15) . . ?
C32 Si1 C31 112.1(5) . . ?
O1 Si1 C33 110.5(2) . . ?
C32 Si1 C33 109.4(3) . . ?
C31 Si1 C33 109.5(5) . . ?
O7 Si2 C64 104.66(14) . . ?
O7 Si2 C66 111.01(18) . . ?
C64 Si2 C66 110.6(2) . . ?
O7 Si2 C65 110.5(2) . . ?
C64 Si2 C65 110.8(3) . . ?
C66 Si2 C65 109.3(3) . . ?
C1 O1 Si1 130.28(18) . . ?
C34 O7 Si2 129.1(2) . . ?
C2 N1 P1 125.5(3) . . ?
C2 N1 P2 124.8(3) . . ?
P1 N1 P2 107.53(11) . . ?
C35 N2 P3 125.0(3) . . ?
C35 N2 P4 124.9(3) . . ?
P3 N2 P4 106.67(12) . . ?
O1 C1 C6 123.8(2) . . ?
O1 C1 C2 117.4(2) . . ?
C6 C1 C2 118.8(2) . . ?
C3 C2 C1 120.4(2) . . ?
C3 C2 N1 121.1(2) . . ?
C1 C2 N1 118.6(2) . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 120.7(3) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 120.6(3) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C8 C7 C12 118.6(4) . . ?
C8 C7 P1 118.5(3) . . ?
C12 C7 P1 122.6(3) . . ?
C7 C8 C9 120.6(4) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C10 119.9(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 119.5(4) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 120.0(4) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C7 121.3(4) . . ?
C11 C12 H12 119.4 . . ?
C7 C12 H12 119.4 . . ?
C14 C13 C18 120.0(4) . . ?
C14 C13 P1 119.1(3) . . ?
C18 C13 P1 120.0(3) . . ?
C13 C14 C15 120.0(4) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 119.9(4) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 120.3(4) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 120.5(4) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C13 119.3(4) . . ?
C17 C18 H18 120.3 . . ?
C13 C18 H18 120.3 . . ?
C24 C19 C20 118.9(4) . . ?
C24 C19 P2 117.8(3) . . ?
C20 C19 P2 123.0(3) . . ?
C21 C20 C19 119.7(4) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C22 C21 C20 120.9(4) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 119.6(4) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 120.5(4) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C19 120.2(4) . . ?
C23 C24 H24 119.9 . . ?
C19 C24 H24 119.9 . . ?
C26 C25 C30 119.7(4) . . ?
C26 C25 P2 119.6(3) . . ?
C30 C25 P2 120.1(3) . . ?
C25 C26 C27 120.0(4) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 119.4(4) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C29 C28 C27 121.0(4) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C30 120.0(4) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 119.9(4) . . ?
C29 C30 H30 120.1 . . ?
C25 C30 H30 120.1 . . ?
Si1 C31 H31A 109.5 . . ?
Si1 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si1 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si1 C32 H32A 109.5 . . ?
Si1 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si1 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si1 C33 H33A 109.5 . . ?
Si1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
Si1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O7 C34 C39 123.6(3) . . ?
O7 C34 C35 118.5(2) . . ?
C39 C34 C35 117.8(3) . . ?
C36 C35 C34 120.3(2) . . ?
C36 C35 N2 120.2(2) . . ?
C34 C35 N2 119.5(2) . . ?
C37 C36 C35 120.7(3) . . ?
C37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C38 C37 C36 119.2(3) . . ?
C38 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?
C39 C38 C37 120.9(3) . . ?
C39 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C38 C39 C34 121.1(3) . . ?
C38 C39 H39 119.5 . . ?
C34 C39 H39 119.5 . . ?
C45 C40 C41 120.0(4) . . ?
C45 C40 P3 125.5(3) . . ?
C41 C40 P3 114.5(3) . . ?
C42 C41 C40 120.0(4) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C43 C42 C41 119.8(4) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C42 C43 C44 120.3(4) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C43 C44 C45 119.9(4) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C40 C45 C44 120.0(4) . . ?
C40 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C51 C46 C47 119.2(4) . . ?
C51 C46 P3 121.6(3) . . ?
C47 C46 P3 118.9(3) . . ?
C48 C47 C46 120.4(4) . . ?
C48 C47 H47 119.8 . . ?
C46 C47 H47 119.8 . . ?
C47 C48 C49 120.1(5) . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C50 C49 C48 119.5(4) . . ?
C50 C49 H49 120.2 . . ?
C48 C49 H49 120.2 . . ?
C49 C50 C51 120.8(4) . . ?
C49 C50 H50 119.6 . . ?
C51 C50 H50 119.6 . . ?
C50 C51 C46 120.0(4) . . ?
C50 C51 H51 120.0 . . ?
C46 C51 H51 120.0 . . ?
C53 C52 C57 119.5(4) . . ?
C53 C52 P4 124.6(3) . . ?
C57 C52 P4 115.6(3) . . ?
C54 C53 C52 119.9(4) . . ?
C54 C53 H53 120.1 . . ?
C52 C53 H53 120.1 . . ?
C55 C54 C53 120.6(4) . . ?
C55 C54 H54 119.7 . . ?
C53 C54 H54 119.7 . . ?
C54 C55 C56 119.9(4) . . ?
C54 C55 H55 120.1 . . ?
C56 C55 H55 120.1 . . ?
C57 C56 C55 119.6(4) . . ?
C57 C56 H56 120.2 . . ?
C55 C56 H56 120.2 . . ?
C56 C57 C52 120.4(4) . . ?
C56 C57 H57 119.8 . . ?
C52 C57 H57 119.8 . . ?
C59 C58 C63 119.6(4) . . ?
C59 C58 P4 121.3(3) . . ?
C63 C58 P4 118.8(3) . . ?
C58 C59 C60 119.1(4) . . ?
C58 C59 H59 120.4 . . ?
C60 C59 H59 120.4 . . ?
C61 C60 C59 121.4(4) . . ?
C61 C60 H60 119.3 . . ?
C59 C60 H60 119.3 . . ?
C60 C61 C62 119.8(4) . . ?
C60 C61 H61 120.1 . . ?
C62 C61 H61 120.1 . . ?
C63 C62 C61 119.6(4) . . ?
C63 C62 H62 120.2 . . ?
C61 C62 H62 120.2 . . ?
C62 C63 C58 120.5(4) . . ?
C62 C63 H63 119.8 . . ?
C58 C63 H63 119.8 . . ?
Si2 C64 H64A 109.5 . . ?
Si2 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
Si2 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
Si2 C65 H65A 109.5 . . ?
Si2 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
Si2 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
Si2 C66 H66A 109.5 . . ?
Si2 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
Si2 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
Cl10 C67 Cl9 111.7(3) . . ?
Cl10 C67 H67A 109.3 . . ?
Cl9 C67 H67A 109.3 . . ?
Cl10 C67 H67B 109.3 . . ?
Cl9 C67 H67B 109.3 . . ?
H67A C67 H67B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl3 Ti1 P1 N1 -179.31(8) . . . . ?
Cl4 Ti1 P1 N1 3.48(13) . . . . ?
Cl1 Ti1 P1 N1 -85.01(8) . . . . ?
Cl2 Ti1 P1 N1 88.23(9) . . . . ?
P2 Ti1 P1 N1 1.11(8) . . . . ?
Cl3 Ti1 P1 C7 -64.97(15) . . . . ?
Cl4 Ti1 P1 C7 117.82(16) . . . . ?
Cl1 Ti1 P1 C7 29.33(15) . . . . ?
Cl2 Ti1 P1 C7 -157.43(15) . . . . ?
P2 Ti1 P1 C7 115.45(15) . . . . ?
Cl3 Ti1 P1 C13 60.79(15) . . . . ?
Cl4 Ti1 P1 C13 -116.42(16) . . . . ?
Cl1 Ti1 P1 C13 155.10(15) . . . . ?
Cl2 Ti1 P1 C13 -31.67(15) . . . . ?
P2 Ti1 P1 C13 -118.78(15) . . . . ?
Cl3 Ti1 P2 N1 -2.10(13) . . . . ?
Cl4 Ti1 P2 N1 179.94(8) . . . . ?
Cl1 Ti1 P2 N1 85.02(8) . . . . ?
Cl2 Ti1 P2 N1 -87.86(8) . . . . ?
P1 Ti1 P2 N1 -1.11(8) . . . . ?
Cl3 Ti1 P2 C19 -116.68(16) . . . . ?
Cl4 Ti1 P2 C19 65.35(15) . . . . ?
Cl1 Ti1 P2 C19 -29.56(15) . . . . ?
Cl2 Ti1 P2 C19 157.56(15) . . . . ?
P1 Ti1 P2 C19 -115.69(15) . . . . ?
Cl3 Ti1 P2 C25 117.36(17) . . . . ?
Cl4 Ti1 P2 C25 -60.61(16) . . . . ?
Cl1 Ti1 P2 C25 -155.53(16) . . . . ?
Cl2 Ti1 P2 C25 31.60(16) . . . . ?
P1 Ti1 P2 C25 118.35(16) . . . . ?
Cl8 Ti2 P3 N2 -2.49(13) . . . . ?
Cl7 Ti2 P3 N2 -178.49(9) . . . . ?
Cl6 Ti2 P3 N2 87.80(9) . . . . ?
Cl5 Ti2 P3 N2 -84.41(9) . . . . ?
P4 Ti2 P3 N2 1.23(8) . . . . ?
Cl8 Ti2 P3 C46 -121.57(17) . . . . ?
Cl7 Ti2 P3 C46 62.43(16) . . . . ?
Cl6 Ti2 P3 C46 -31.29(16) . . . . ?
Cl5 Ti2 P3 C46 156.51(16) . . . . ?
P4 Ti2 P3 C46 -117.85(16) . . . . ?
Cl8 Ti2 P3 C40 113.61(18) . . . . ?
Cl7 Ti2 P3 C40 -62.39(16) . . . . ?
Cl6 Ti2 P3 C40 -156.11(16) . . . . ?
Cl5 Ti2 P3 C40 31.69(16) . . . . ?
P4 Ti2 P3 C40 117.33(16) . . . . ?
Cl8 Ti2 P4 N2 177.10(9) . . . . ?
Cl7 Ti2 P4 N2 -0.57(14) . . . . ?
Cl6 Ti2 P4 N2 -88.74(9) . . . . ?
Cl5 Ti2 P4 N2 82.68(9) . . . . ?
P3 Ti2 P4 N2 -1.23(8) . . . . ?
Cl8 Ti2 P4 C52 61.74(16) . . . . ?
Cl7 Ti2 P4 C52 -115.93(18) . . . . ?
Cl6 Ti2 P4 C52 155.91(16) . . . . ?
Cl5 Ti2 P4 C52 -32.68(16) . . . . ?
P3 Ti2 P4 C52 -116.58(16) . . . . ?
Cl8 Ti2 P4 C58 -65.17(16) . . . . ?
Cl7 Ti2 P4 C58 117.17(18) . . . . ?
Cl6 Ti2 P4 C58 29.00(16) . . . . ?
Cl5 Ti2 P4 C58 -159.59(16) . . . . ?
P3 Ti2 P4 C58 116.51(16) . . . . ?
C32 Si1 O1 C1 62.5(6) . . . . ?
C31 Si1 O1 C1 -176.5(7) . . . . ?
C33 Si1 O1 C1 -58.7(5) . . . . ?
C64 Si2 O7 C34 -175.5(4) . . . . ?
C66 Si2 O7 C34 -56.2(4) . . . . ?
C65 Si2 O7 C34 65.2(4) . . . . ?
C7 P1 N1 C2 71.5(2) . . . . ?
C13 P1 N1 C2 -37.5(3) . . . . ?
Ti1 P1 N1 C2 -165.6(2) . . . . ?
C7 P1 N1 P2 -124.46(15) . . . . ?
C13 P1 N1 P2 126.50(17) . . . . ?
Ti1 P1 N1 P2 -1.60(11) . . . . ?
C19 P2 N1 C2 -72.5(2) . . . . ?
C25 P2 N1 C2 37.2(3) . . . . ?
Ti1 P2 N1 C2 165.7(2) . . . . ?
C19 P2 N1 P1 123.40(15) . . . . ?
C25 P2 N1 P1 -126.94(17) . . . . ?
Ti1 P2 N1 P1 1.59(11) . . . . ?
C46 P3 N2 C35 -29.0(3) . . . . ?
C40 P3 N2 C35 77.6(3) . . . . ?
Ti2 P3 N2 C35 -161.8(2) . . . . ?
C46 P3 N2 P4 131.04(16) . . . . ?
C40 P3 N2 P4 -122.33(17) . . . . ?
Ti2 P3 N2 P4 -1.75(11) . . . . ?
C52 P4 N2 C35 -78.8(3) . . . . ?
C58 P4 N2 C35 29.4(3) . . . . ?
Ti2 P4 N2 C35 161.8(2) . . . . ?
C52 P4 N2 P3 121.07(17) . . . . ?
C58 P4 N2 P3 -130.66(16) . . . . ?
Ti2 P4 N2 P3 1.75(11) . . . . ?
Si1 O1 C1 C6 0.8(8) . . . . ?
Si1 O1 C1 C2 -178.6(4) . . . . ?
O1 C1 C2 C3 -180.0(5) . . . . ?
C6 C1 C2 C3 0.6(7) . . . . ?
O1 C1 C2 N1 -0.2(6) . . . . ?
C6 C1 C2 N1 -179.7(5) . . . . ?
P1 N1 C2 C3 -99.1(4) . . . . ?
P2 N1 C2 C3 99.6(4) . . . . ?
P1 N1 C2 C1 81.2(5) . . . . ?
P2 N1 C2 C1 -80.2(5) . . . . ?
C1 C2 C3 C4 0.3(7) . . . . ?
N1 C2 C3 C4 -179.4(4) . . . . ?
C2 C3 C4 C5 -0.6(8) . . . . ?
C3 C4 C5 C6 0.0(8) . . . . ?
C4 C5 C6 C1 0.9(8) . . . . ?
O1 C1 C6 C5 179.4(5) . . . . ?
C2 C1 C6 C5 -1.2(8) . . . . ?
N1 P1 C7 C8 -152.9(3) . . . . ?
C13 P1 C7 C8 -35.6(3) . . . . ?
Ti1 P1 C7 C8 100.5(3) . . . . ?
N1 P1 C7 C12 33.3(3) . . . . ?
C13 P1 C7 C12 150.5(3) . . . . ?
Ti1 P1 C7 C12 -73.3(3) . . . . ?
C12 C7 C8 C9 1.1(6) . . . . ?
P1 C7 C8 C9 -172.9(3) . . . . ?
C7 C8 C9 C10 -0.8(6) . . . . ?
C8 C9 C10 C11 -0.6(7) . . . . ?
C9 C10 C11 C12 1.7(6) . . . . ?
C10 C11 C12 C7 -1.4(6) . . . . ?
C8 C7 C12 C11 -0.1(6) . . . . ?
P1 C7 C12 C11 173.8(3) . . . . ?
N1 P1 C13 C14 -134.9(3) . . . . ?
C7 P1 C13 C14 110.4(4) . . . . ?
Ti1 P1 C13 C14 -23.6(4) . . . . ?
N1 P1 C13 C18 55.9(4) . . . . ?
C7 P1 C13 C18 -58.8(3) . . . . ?
Ti1 P1 C13 C18 167.2(3) . . . . ?
C18 C13 C14 C15 0.3(6) . . . . ?
P1 C13 C14 C15 -168.9(3) . . . . ?
C13 C14 C15 C16 -0.7(7) . . . . ?
C14 C15 C16 C17 0.3(8) . . . . ?
C15 C16 C17 C18 0.6(7) . . . . ?
C16 C17 C18 C13 -1.0(7) . . . . ?
C14 C13 C18 C17 0.5(6) . . . . ?
P1 C13 C18 C17 169.6(3) . . . . ?
N1 P2 C19 C24 157.9(3) . . . . ?
C25 P2 C19 C24 40.7(3) . . . . ?
Ti1 P2 C19 C24 -95.9(3) . . . . ?
N1 P2 C19 C20 -28.3(3) . . . . ?
C25 P2 C19 C20 -145.5(3) . . . . ?
Ti1 P2 C19 C20 77.9(3) . . . . ?
C24 C19 C20 C21 1.5(6) . . . . ?
P2 C19 C20 C21 -172.2(3) . . . . ?
C19 C20 C21 C22 0.4(6) . . . . ?
C20 C21 C22 C23 -1.6(7) . . . . ?
C21 C22 C23 C24 0.9(7) . . . . ?
C22 C23 C24 C19 0.9(7) . . . . ?
C20 C19 C24 C23 -2.1(6) . . . . ?
P2 C19 C24 C23 171.9(3) . . . . ?
N1 P2 C25 C26 131.7(3) . . . . ?
C19 P2 C25 C26 -112.8(4) . . . . ?
Ti1 P2 C25 C26 20.7(4) . . . . ?
N1 P2 C25 C30 -56.7(4) . . . . ?
C19 P2 C25 C30 58.7(4) . . . . ?
Ti1 P2 C25 C30 -167.7(3) . . . . ?
C30 C25 C26 C27 1.2(7) . . . . ?
P2 C25 C26 C27 172.7(3) . . . . ?
C25 C26 C27 C28 0.3(7) . . . . ?
C26 C27 C28 C29 -1.2(7) . . . . ?
C27 C28 C29 C30 0.6(7) . . . . ?
C28 C29 C30 C25 0.9(7) . . . . ?
C26 C25 C30 C29 -1.8(6) . . . . ?
P2 C25 C30 C29 -173.3(3) . . . . ?
Si2 O7 C34 C39 -3.8(6) . . . . ?
Si2 O7 C34 C35 176.4(3) . . . . ?
O7 C34 C35 C36 -178.0(4) . . . . ?
C39 C34 C35 C36 2.2(7) . . . . ?
O7 C34 C35 N2 1.5(6) . . . . ?
C39 C34 C35 N2 -178.3(4) . . . . ?
P3 N2 C35 C36 -104.4(4) . . . . ?
P4 N2 C35 C36 99.1(4) . . . . ?
P3 N2 C35 C34 76.1(5) . . . . ?
P4 N2 C35 C34 -80.4(5) . . . . ?
C34 C35 C36 C37 -1.0(7) . . . . ?
N2 C35 C36 C37 179.4(5) . . . . ?
C35 C36 C37 C38 -0.6(8) . . . . ?
C36 C37 C38 C39 1.0(8) . . . . ?
C37 C38 C39 C34 0.2(8) . . . . ?
O7 C34 C39 C38 178.5(4) . . . . ?
C35 C34 C39 C38 -1.8(7) . . . . ?
N2 P3 C40 C45 2.2(4) . . . . ?
C46 P3 C40 C45 116.1(4) . . . . ?
Ti2 P3 C40 C45 -105.0(3) . . . . ?
N2 P3 C40 C41 -176.7(3) . . . . ?
C46 P3 C40 C41 -62.8(3) . . . . ?
Ti2 P3 C40 C41 76.1(3) . . . . ?
C45 C40 C41 C42 -0.6(7) . . . . ?
P3 C40 C41 C42 178.3(4) . . . . ?
C40 C41 C42 C43 0.2(7) . . . . ?
C41 C42 C43 C44 -0.4(7) . . . . ?
C42 C43 C44 C45 1.0(6) . . . . ?
C41 C40 C45 C44 1.3(6) . . . . ?
P3 C40 C45 C44 -177.5(3) . . . . ?
C43 C44 C45 C40 -1.5(6) . . . . ?
N2 P3 C46 C51 -120.2(3) . . . . ?
C40 P3 C46 C51 124.7(4) . . . . ?
Ti2 P3 C46 C51 -7.3(4) . . . . ?
N2 P3 C46 C47 65.4(3) . . . . ?
C40 P3 C46 C47 -49.7(4) . . . . ?
Ti2 P3 C46 C47 178.3(3) . . . . ?
C51 C46 C47 C48 0.9(6) . . . . ?
P3 C46 C47 C48 175.5(3) . . . . ?
C46 C47 C48 C49 -0.4(7) . . . . ?
C47 C48 C49 C50 0.2(8) . . . . ?
C48 C49 C50 C51 -0.7(8) . . . . ?
C49 C50 C51 C46 1.3(8) . . . . ?
C47 C46 C51 C50 -1.4(6) . . . . ?
P3 C46 C51 C50 -175.8(4) . . . . ?
N2 P4 C52 C53 -19.0(4) . . . . ?
C58 P4 C52 C53 -132.8(3) . . . . ?
Ti2 P4 C52 C53 87.1(3) . . . . ?
N2 P4 C52 C57 167.1(3) . . . . ?
C58 P4 C52 C57 53.3(3) . . . . ?
Ti2 P4 C52 C57 -86.7(3) . . . . ?
C57 C52 C53 C54 -2.2(6) . . . . ?
P4 C52 C53 C54 -175.8(3) . . . . ?
C52 C53 C54 C55 2.9(6) . . . . ?
C53 C54 C55 C56 -1.4(6) . . . . ?
C54 C55 C56 C57 -0.8(7) . . . . ?
C55 C56 C57 C52 1.5(7) . . . . ?
C53 C52 C57 C56 0.0(6) . . . . ?
P4 C52 C57 C56 174.2(3) . . . . ?
N2 P4 C58 C59 121.5(3) . . . . ?
C52 P4 C58 C59 -123.1(3) . . . . ?
Ti2 P4 C58 C59 9.7(4) . . . . ?
N2 P4 C58 C63 -64.3(4) . . . . ?
C52 P4 C58 C63 51.2(4) . . . . ?
Ti2 P4 C58 C63 -176.0(3) . . . . ?
C63 C58 C59 C60 2.7(6) . . . . ?
P4 C58 C59 C60 176.9(4) . . . . ?
C58 C59 C60 C61 -0.6(8) . . . . ?
C59 C60 C61 C62 -1.6(9) . . . . ?
C60 C61 C62 C63 1.7(8) . . . . ?
C61 C62 C63 C58 0.5(7) . . . . ?
C59 C58 C63 C62 -2.7(7) . . . . ?
P4 C58 C63 C62 -177.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.919
_diffrn_reflns_theta_full        30.86
_diffrn_measured_fraction_theta_full 0.919
_refine_diff_density_max         0.825
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.097
_database_code_depnum_ccdc_archive 'CCDC 995244'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_d:\30js26

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H25 N O P2'
_chemical_formula_weight         477.45

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'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 '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
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   8.701(2)
_cell_length_b                   10.6660(10)
_cell_length_c                   13.9380(13)
_cell_angle_alpha                70.2480(10)
_cell_angle_beta                 84.203(3)
_cell_angle_gamma                81.578(3)
_cell_volume                     1202.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22129
_cell_measurement_theta_min      1.55
_cell_measurement_theta_max      30.86

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             500
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Low data completion ratio is due to the limitations of the instrument available
at the Australian Synchrotron operating under rotation data collection with a
fixed detector and affects some high angle data. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Synchrotron ID'
_diffrn_radiation_monochromator  Si<111>
_diffrn_measurement_device_type  '3-ID1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_detector_area_resol_mean 'ADSC Q315'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25361
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         30.86
_reflns_number_total             6695
_reflns_number_gt                6170
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       BLU-ICE
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)' 
;
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The H attached to P was located and refined in x,y,z. All other Hs 
were calculated and allowed to ride with their C atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0534P)²+0.8283P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6695
_refine_ls_number_parameters     310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1145
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
P1 P 0.37987(4) 0.74208(3) 0.16562(2) 0.01216(8) Uani 1 1 d . . .
P2 P 0.48450(4) 0.96550(3) 0.21675(2) 0.01332(8) Uani 1 1 d . . .
O1 O 0.30936(12) 0.61033(9) 0.26852(7) 0.01556(18) Uani 1 1 d . . .
N1 N 0.40166(13) 0.81798(10) 0.25511(8) 0.01304(19) Uani 1 1 d . . .
C1 C 0.30514(16) 0.62582(12) 0.36108(9) 0.0142(2) Uani 1 1 d . . .
C2 C 0.35665(15) 0.74556(11) 0.35691(9) 0.0133(2) Uani 1 1 d . . .
C3 C 0.35644(16) 0.77787(12) 0.44532(9) 0.0164(2) Uani 1 1 d . . .
H3 H 0.3902 0.8595 0.4433 0.020 Uiso 1 1 calc R . .
C4 C 0.30524(18) 0.68723(14) 0.53764(10) 0.0196(3) Uani 1 1 d . . .
H4 H 0.3040 0.7080 0.5989 0.024 Uiso 1 1 calc R . .
C5 C 0.25613(19) 0.56729(14) 0.54126(10) 0.0212(3) Uani 1 1 d . . .
H5 H 0.2233 0.5066 0.6049 0.025 Uiso 1 1 calc R . .
C6 C 0.25464(17) 0.53518(13) 0.45190(10) 0.0185(3) Uani 1 1 d . . .
H6 H 0.2201 0.4539 0.4536 0.022 Uiso 1 1 calc R . .
C7 C 0.20348(16) 0.76966(12) 0.09661(9) 0.0145(2) Uani 1 1 d . . .
C8 C 0.07591(17) 0.69735(13) 0.13355(10) 0.0183(2) Uani 1 1 d . . .
H8 H 0.0770 0.6304 0.1990 0.022 Uiso 1 1 calc R . .
C9 C -0.05227(18) 0.72288(15) 0.07505(11) 0.0212(3) Uani 1 1 d . . .
H9 H -0.1391 0.6744 0.1014 0.025 Uiso 1 1 calc R . .
C10 C -0.05481(18) 0.81855(14) -0.02158(11) 0.0217(3) Uani 1 1 d . . .
H10 H -0.1426 0.8350 -0.0614 0.026 Uiso 1 1 calc R . .
C11 C 0.07178(18) 0.89013(14) -0.05985(11) 0.0217(3) Uani 1 1 d . . .
H11 H 0.0714 0.9547 -0.1264 0.026 Uiso 1 1 calc R . .
C12 C 0.19898(17) 0.86696(12) -0.00053(10) 0.0180(2) Uani 1 1 d . . .
H12 H 0.2839 0.9179 -0.0263 0.022 Uiso 1 1 calc R . .
C13 C 0.52887(16) 0.62321(12) 0.13069(9) 0.0139(2) Uani 1 1 d . . .
C14 C 0.59577(17) 0.50573(13) 0.20152(10) 0.0187(3) Uani 1 1 d . . .
H14 H 0.5635 0.4842 0.2718 0.022 Uiso 1 1 calc R . .
C15 C 0.70969(18) 0.42004(14) 0.16939(11) 0.0222(3) Uani 1 1 d . . .
H15 H 0.7569 0.3416 0.2182 0.027 Uiso 1 1 calc R . .
C16 C 0.75475(18) 0.44858(14) 0.06649(11) 0.0217(3) Uani 1 1 d . . .
H16 H 0.8309 0.3889 0.0447 0.026 Uiso 1 1 calc R . .
C17 C 0.68804(18) 0.56474(14) -0.00431(10) 0.0208(3) Uani 1 1 d . . .
H17 H 0.7177 0.5841 -0.0748 0.025 Uiso 1 1 calc R . .
C18 C 0.57787(17) 0.65309(13) 0.02760(10) 0.0178(2) Uani 1 1 d . . .
H18 H 0.5357 0.7342 -0.0210 0.021 Uiso 1 1 calc R . .
C19 C 0.33778(16) 1.07882(12) 0.26001(9) 0.0148(2) Uani 1 1 d . . .
C20 C 0.18217(17) 1.05632(12) 0.27981(10) 0.0179(2) Uani 1 1 d . . .
H20 H 0.1523 0.9741 0.2799 0.021 Uiso 1 1 calc R . .
C21 C 0.07000(18) 1.15350(14) 0.29945(11) 0.0224(3) Uani 1 1 d . . .
H21 H -0.0359 1.1374 0.3125 0.027 Uiso 1 1 calc R . .
C22 C 0.1126(2) 1.27395(14) 0.29999(11) 0.0244(3) Uani 1 1 d . . .
H22 H 0.0361 1.3397 0.3139 0.029 Uiso 1 1 calc R . .
C23 C 0.2665(2) 1.29777(13) 0.28020(11) 0.0230(3) Uani 1 1 d . . .
H23 H 0.2957 1.3798 0.2810 0.028 Uiso 1 1 calc R . .
C24 C 0.37919(18) 1.20163(12) 0.25913(10) 0.0188(3) Uani 1 1 d . . .
H24 H 0.4844 1.2194 0.2441 0.023 Uiso 1 1 calc R . .
C25 C 0.64011(16) 0.92217(12) 0.30623(9) 0.0153(2) Uani 1 1 d . . .
C26 C 0.65101(18) 0.97544(14) 0.38402(10) 0.0196(3) Uani 1 1 d . . .
H26 H 0.5713 1.0410 0.3950 0.024 Uiso 1 1 calc R . .
C27 C 0.77783(19) 0.93304(15) 0.44541(11) 0.0235(3) Uani 1 1 d . . .
H27 H 0.7835 0.9694 0.4983 0.028 Uiso 1 1 calc R . .
C28 C 0.89621(19) 0.83797(15) 0.43004(11) 0.0233(3) Uani 1 1 d . . .
H28 H 0.9825 0.8092 0.4722 0.028 Uiso 1 1 calc R . .
C29 C 0.88709(19) 0.78532(15) 0.35244(12) 0.0248(3) Uani 1 1 d . . .
H29 H 0.9672 0.7199 0.3417 0.030 Uiso 1 1 calc R . .
H1 H 0.434(2) 0.8471(18) 0.0936(14) 0.016 Uiso 1 1 d . . .
C30 C 0.76146(18) 0.82789(14) 0.29062(11) 0.0218(3) Uani 1 1 d . . .
H30 H 0.7576 0.7926 0.2369 0.026 Uiso 1 1 calc R . .


_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 N1 1.7384(11) . ?
P1 O1 1.7666(9) . ?
P1 C13 1.8259(13) . ?
P1 C7 1.8281(14) . ?
P1 H1 1.337(18) . ?
P2 N1 1.7225(11) . ?
P2 C19 1.8274(13) . ?
P2 C25 1.8360(14) . ?
O1 C1 1.3511(14) . ?
N1 C2 1.4137(15) . ?
C1 C6 1.3838(17) . ?
C1 C2 1.3956(17) . ?
C2 C3 1.3870(16) . ?
C3 C4 1.3994(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.4005(18) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.3997(19) . ?
C7 C12 1.4003(17) . ?
C8 C9 1.388(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.391(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.3963(17) . ?
C13 C18 1.3981(17) . ?
C14 C15 1.3929(19) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.387(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.3919(18) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.394(2) . ?
C19 C24 1.4044(17) . ?
C20 C21 1.3940(19) . ?
C20 H20 0.9500 . ?
C21 C22 1.391(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3962(19) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.4000(17) . ?
C25 C30 1.4014(19) . ?
C26 C27 1.392(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(2) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 O1 86.76(5) . . ?
N1 P1 C13 124.18(6) . . ?
O1 P1 C13 90.53(5) . . ?
N1 P1 C7 124.01(6) . . ?
O1 P1 C7 92.22(5) . . ?
C13 P1 C7 111.81(6) . . ?
N1 P1 H1 88.3(8) . . ?
O1 P1 H1 175.1(8) . . ?
C13 P1 H1 92.4(8) . . ?
C7 P1 H1 90.4(8) . . ?
N1 P2 C19 102.99(6) . . ?
N1 P2 C25 101.11(6) . . ?
C19 P2 C25 105.06(6) . . ?
C1 O1 P1 115.18(8) . . ?
C2 N1 P2 125.37(8) . . ?
C2 N1 P1 115.10(8) . . ?
P2 N1 P1 119.40(6) . . ?
O1 C1 C6 124.96(11) . . ?
O1 C1 C2 112.96(10) . . ?
C6 C1 C2 122.08(11) . . ?
C3 C2 C1 120.10(11) . . ?
C3 C2 N1 129.91(11) . . ?
C1 C2 N1 109.99(10) . . ?
C2 C3 C4 118.38(12) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 121.11(12) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 120.59(12) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 117.74(12) . . ?
C1 C6 H6 121.1 . . ?
C5 C6 H6 121.1 . . ?
C8 C7 C12 118.50(12) . . ?
C8 C7 P1 124.17(10) . . ?
C12 C7 P1 117.31(10) . . ?
C9 C8 C7 120.40(12) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C10 C9 C8 120.62(14) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 119.67(14) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C10 C11 C12 119.87(13) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C7 120.91(13) . . ?
C11 C12 H12 119.5 . . ?
C7 C12 H12 119.5 . . ?
C14 C13 C18 119.05(12) . . ?
C14 C13 P1 123.32(9) . . ?
C18 C13 P1 117.63(9) . . ?
C15 C14 C13 120.17(12) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 120.43(13) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 119.65(13) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 120.23(12) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C13 120.40(12) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C20 C19 C24 118.81(12) . . ?
C20 C19 P2 122.17(9) . . ?
C24 C19 P2 118.39(11) . . ?
C19 C20 C21 120.53(12) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C22 C21 C20 120.20(15) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C21 119.90(13) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.22(13) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 120.33(14) . . ?
C23 C24 H24 119.8 . . ?
C19 C24 H24 119.8 . . ?
C26 C25 C30 118.29(13) . . ?
C26 C25 P2 127.22(10) . . ?
C30 C25 P2 114.46(10) . . ?
C27 C26 C25 120.49(13) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C28 C27 C26 120.58(13) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 119.35(14) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C30 C29 C28 120.28(14) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C25 120.98(13) . . ?
C29 C30 H30 119.5 . . ?
C25 C30 H30 119.5 . . ?

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
N1 P1 O1 C1 -0.26(10) . . . . ?
C13 P1 O1 C1 123.94(10) . . . . ?
C7 P1 O1 C1 -124.21(9) . . . . ?
C19 P2 N1 C2 -59.28(12) . . . . ?
C25 P2 N1 C2 49.21(12) . . . . ?
C19 P2 N1 P1 124.96(7) . . . . ?
C25 P2 N1 P1 -126.55(7) . . . . ?
O1 P1 N1 C2 -0.18(9) . . . . ?
C13 P1 N1 C2 -88.63(11) . . . . ?
C7 P1 N1 C2 90.32(10) . . . . ?
O1 P1 N1 P2 176.00(8) . . . . ?
C13 P1 N1 P2 87.55(9) . . . . ?
C7 P1 N1 P2 -93.50(9) . . . . ?
P1 O1 C1 C6 -179.84(11) . . . . ?
P1 O1 C1 C2 0.64(14) . . . . ?
O1 C1 C2 C3 178.66(12) . . . . ?
C6 C1 C2 C3 -0.9(2) . . . . ?
O1 C1 C2 N1 -0.74(16) . . . . ?
C6 C1 C2 N1 179.73(12) . . . . ?
P2 N1 C2 C3 5.3(2) . . . . ?
P1 N1 C2 C3 -178.77(12) . . . . ?
P2 N1 C2 C1 -175.36(10) . . . . ?
P1 N1 C2 C1 0.56(14) . . . . ?
C1 C2 C3 C4 0.7(2) . . . . ?
N1 C2 C3 C4 179.93(13) . . . . ?
C2 C3 C4 C5 0.2(2) . . . . ?
C3 C4 C5 C6 -0.9(2) . . . . ?
O1 C1 C6 C5 -179.31(13) . . . . ?
C2 C1 C6 C5 0.2(2) . . . . ?
C4 C5 C6 C1 0.7(2) . . . . ?
N1 P1 C7 C8 -86.42(12) . . . . ?
O1 P1 C7 C8 1.18(11) . . . . ?
C13 P1 C7 C8 92.65(11) . . . . ?
N1 P1 C7 C12 95.47(10) . . . . ?
O1 P1 C7 C12 -176.94(10) . . . . ?
C13 P1 C7 C12 -85.47(10) . . . . ?
C12 C7 C8 C9 -0.50(18) . . . . ?
P1 C7 C8 C9 -178.60(10) . . . . ?
C7 C8 C9 C10 1.2(2) . . . . ?
C8 C9 C10 C11 -0.4(2) . . . . ?
C9 C10 C11 C12 -1.0(2) . . . . ?
C10 C11 C12 C7 1.7(2) . . . . ?
C8 C7 C12 C11 -0.96(19) . . . . ?
P1 C7 C12 C11 177.27(10) . . . . ?
N1 P1 C13 C14 55.74(14) . . . . ?
O1 P1 C13 C14 -30.71(12) . . . . ?
C7 P1 C13 C14 -123.32(12) . . . . ?
N1 P1 C13 C18 -123.89(10) . . . . ?
O1 P1 C13 C18 149.66(11) . . . . ?
C7 P1 C13 C18 57.05(12) . . . . ?
C18 C13 C14 C15 0.0(2) . . . . ?
P1 C13 C14 C15 -179.59(11) . . . . ?
C13 C14 C15 C16 -1.8(2) . . . . ?
C14 C15 C16 C17 1.4(2) . . . . ?
C15 C16 C17 C18 0.8(2) . . . . ?
C16 C17 C18 C13 -2.5(2) . . . . ?
C14 C13 C18 C17 2.1(2) . . . . ?
P1 C13 C18 C17 -178.26(11) . . . . ?
N1 P2 C19 C20 -21.47(12) . . . . ?
C25 P2 C19 C20 -126.95(11) . . . . ?
N1 P2 C19 C24 167.76(10) . . . . ?
C25 P2 C19 C24 62.28(11) . . . . ?
C24 C19 C20 C21 -0.67(19) . . . . ?
P2 C19 C20 C21 -171.41(10) . . . . ?
C19 C20 C21 C22 -0.3(2) . . . . ?
C20 C21 C22 C23 0.5(2) . . . . ?
C21 C22 C23 C24 0.4(2) . . . . ?
C22 C23 C24 C19 -1.4(2) . . . . ?
C20 C19 C24 C23 1.52(19) . . . . ?
P2 C19 C24 C23 172.61(10) . . . . ?
N1 P2 C25 C26 -112.82(12) . . . . ?
C19 P2 C25 C26 -5.96(14) . . . . ?
N1 P2 C25 C30 69.15(11) . . . . ?
C19 P2 C25 C30 176.02(10) . . . . ?
C30 C25 C26 C27 -1.4(2) . . . . ?
P2 C25 C26 C27 -179.38(11) . . . . ?
C25 C26 C27 C28 0.5(2) . . . . ?
C26 C27 C28 C29 0.1(2) . . . . ?
C27 C28 C29 C30 0.4(2) . . . . ?
C28 C29 C30 C25 -1.3(2) . . . . ?
C26 C25 C30 C29 1.9(2) . . . . ?
P2 C25 C30 C29 -179.93(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.883
_diffrn_reflns_theta_full        30.86
_diffrn_measured_fraction_theta_full 0.883
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 995245'
