# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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.
# 
#  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_x0349fin

_audit_creation_date             2007-12-07T23:32:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C68 H96 N4 O2 P4'
_chemical_formula_weight         1125.37

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   32.6565(13)
_cell_length_b                   12.9533(4)
_cell_length_c                   16.2958(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.974(3)
_cell_angle_gamma                90
_cell_volume                     6627.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    5409
_cell_measurement_theta_min      2.5562
_cell_measurement_theta_max      28.7279

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

_exptl_crystal_description       needles
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2432
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.97401
_exptl_absorpt_correction_T_max  1

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

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_orient_matrix_ub_11      -0.0315041975
_diffrn_orient_matrix_ub_12      -0.0301651826
_diffrn_orient_matrix_ub_13      0.0061550662
_diffrn_orient_matrix_ub_21      -0.0244718152
_diffrn_orient_matrix_ub_22      0.001416774
_diffrn_orient_matrix_ub_23      -0.0211876639
_diffrn_orient_matrix_ub_31      0.020066569
_diffrn_orient_matrix_ub_32      -0.0456251437
_diffrn_orient_matrix_ub_33      -0.0047308518
_diffrn_measurement_device_type  'ccd Xcalibur S'
_diffrn_measurement_method       'ω- amd φ-scans'
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_number            30265
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.6
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_full        23.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             4752
_reflns_number_gt                2605
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'Bruker SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX - Version 1.64.05 (Farrugia, 1999)'

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

_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)+(0.0729P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4752
_refine_ls_number_parameters     423
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1195
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.946
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.04

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.36126(3) 0.13654(9) 0.25204(6) 0.0604(4) Uani 1 1 d D . .
P2 P 0.42572(3) 0.23525(7) 0.05195(5) 0.0473(3) Uani 1 1 d D . .
N1 N 0.38048(8) 0.0906(2) 0.10669(16) 0.0436(8) Uani 1 1 d . . .
C1 C 0.35115(11) 0.1593(3) 0.1354(2) 0.0588(11) Uani 1 1 d . A .
H1A H 0.3212 0.1428 0.1051 0.071 Uiso 1 1 calc R . .
H1B H 0.3567 0.2323 0.1242 0.071 Uiso 1 1 calc R . .
C2 C 0.38776(10) 0.1267(3) 0.02669(19) 0.0424(9) Uani 1 1 d . A .
H2A H 0.3606 0.1496 -0.0132 0.051 Uiso 1 1 calc R . .
H2B H 0.3996 0.0701 -0.0007 0.051 Uiso 1 1 calc R . .
C3 C 0.47587(10) 0.1630(2) 0.0845(2) 0.0439(9) Uani 1 1 d . A .
H3A H 0.473 0.1076 0.1244 0.053 Uiso 1 1 calc R . .
H3B H 0.4808 0.1296 0.0335 0.053 Uiso 1 1 calc R . .
C4 C 0.51429(12) 0.2279(3) 0.1269(2) 0.0478(10) Uani 1 1 d . . .
H4A H 0.5085 0.2667 0.1749 0.057 Uiso 1 1 calc R A .
H4B H 0.5193 0.2787 0.0853 0.057 Uiso 1 1 calc R . .
C5 C 0.55405(11) 0.1622(3) 0.1603(2) 0.0484(10) Uani 1 1 d . A .
H5A H 0.5485 0.1106 0.2008 0.058 Uiso 1 1 calc R . .
H5B H 0.5597 0.1242 0.1119 0.058 Uiso 1 1 calc R . .
C6 C 0.59342(11) 0.2238(3) 0.2047(2) 0.0581(11) Uani 1 1 d . . .
H6A H 0.5877 0.2647 0.2517 0.07 Uiso 1 1 calc R A .
H6B H 0.6005 0.2723 0.1637 0.07 Uiso 1 1 calc R . .
C7 C 0.32003(19) 0.2136(5) 0.2838(4) 0.046(2) Uani 0.629(3) 1 d PD A 1
C8 C 0.2976(3) 0.1528(6) 0.3275(5) 0.053(3) Uani 0.629(3) 1 d PD A 1
C9 C 0.26621(19) 0.1968(6) 0.3593(4) 0.060(2) Uani 0.629(3) 1 d PD A 1
H9 H 0.2518 0.1554 0.3907 0.072 Uiso 0.629(3) 1 calc PR A 1
C10 C 0.2557(2) 0.2999(7) 0.3459(4) 0.074(2) Uani 0.629(3) 1 d PD A 1
C11 C 0.2772(2) 0.3582(6) 0.3020(4) 0.071(2) Uani 0.629(3) 1 d PD A 1
H11 H 0.27 0.4291 0.2927 0.086 Uiso 0.629(3) 1 calc PR A 1
C12 C 0.3092(2) 0.3186(6) 0.2705(4) 0.054(2) Uani 0.629(3) 1 d PD A 1
C13 C 0.3075(4) 0.0393(6) 0.3457(8) 0.062(3) Uani 0.629(3) 1 d PD A 1
H13A H 0.2867 0.0094 0.3723 0.093 Uiso 0.629(3) 1 calc PR A 1
H13B H 0.3362 0.032 0.3844 0.093 Uiso 0.629(3) 1 calc PR A 1
H13C H 0.3059 0.0032 0.2921 0.093 Uiso 0.629(3) 1 calc PR A 1
C14 C 0.2208(2) 0.3470(8) 0.3808(5) 0.117(3) Uani 0.629(3) 1 d PD A 1
H14A H 0.2304 0.4141 0.4068 0.176 Uiso 0.629(3) 1 calc PR A 1
H14B H 0.215 0.3008 0.4239 0.176 Uiso 0.629(3) 1 calc PR A 1
H14C H 0.1948 0.3562 0.3341 0.176 Uiso 0.629(3) 1 calc PR A 1
C15 C 0.3298(2) 0.3914(6) 0.2215(5) 0.072(2) Uani 0.629(3) 1 d PD A 1
H15A H 0.3256 0.3655 0.1633 0.108 Uiso 0.629(3) 1 calc PR A 1
H15B H 0.3604 0.3961 0.25 0.108 Uiso 0.629(3) 1 calc PR A 1
H15C H 0.3169 0.46 0.2195 0.108 Uiso 0.629(3) 1 calc PR A 1
C7F C 0.3092(3) 0.1651(9) 0.2761(7) 0.046(2) Uani 0.371(3) 1 d PD A 2
C8F C 0.2918(5) 0.0991(11) 0.3256(10) 0.053(3) Uani 0.371(3) 1 d PD A 2
C9F C 0.2561(3) 0.1285(9) 0.3514(7) 0.060(2) Uani 0.371(3) 1 d PD A 2
H9F H 0.2443 0.0822 0.3839 0.072 Uiso 0.371(3) 1 calc PR A 2
C10F C 0.2380(4) 0.2247(9) 0.3299(7) 0.074(2) Uani 0.371(3) 1 d PD A 2
C11F C 0.2553(3) 0.2903(9) 0.2805(6) 0.071(2) Uani 0.371(3) 1 d PD A 2
H11F H 0.2427 0.3562 0.265 0.086 Uiso 0.371(3) 1 calc PR A 2
C12F C 0.2904(3) 0.2614(9) 0.2534(6) 0.054(2) Uani 0.371(3) 1 d PD A 2
C13F C 0.3086(8) -0.0057(12) 0.3525(15) 0.062(3) Uani 0.371(3) 1 d PD A 2
H13D H 0.292 -0.0371 0.3878 0.093 Uiso 0.371(3) 1 calc PR A 2
H13E H 0.3385 -0.0007 0.3857 0.093 Uiso 0.371(3) 1 calc PR A 2
H13F H 0.3063 -0.0485 0.3019 0.093 Uiso 0.371(3) 1 calc PR A 2
C14F C 0.1984(4) 0.2579(14) 0.3577(9) 0.117(3) Uani 0.371(3) 1 d PD A 2
H14D H 0.1951 0.2123 0.4034 0.176 Uiso 0.371(3) 1 calc PR A 2
H14E H 0.1731 0.2531 0.3089 0.176 Uiso 0.371(3) 1 calc PR A 2
H14F H 0.202 0.3292 0.3785 0.176 Uiso 0.371(3) 1 calc PR A 2
C15F C 0.3062(4) 0.3412(10) 0.2021(9) 0.072(2) Uani 0.371(3) 1 d PD A 2
H15D H 0.2957 0.3246 0.1412 0.108 Uiso 0.371(3) 1 calc PR A 2
H15E H 0.3374 0.3415 0.219 0.108 Uiso 0.371(3) 1 calc PR A 2
H15F H 0.2957 0.4095 0.2126 0.108 Uiso 0.371(3) 1 calc PR A 2
C16 C 0.4301(3) 0.2948(11) -0.0491(6) 0.0449(12) Uani 0.629(3) 1 d PD A 1
C17 C 0.4426(3) 0.3992(11) -0.0455(7) 0.050(3) Uani 0.629(3) 1 d PD A 1
C18 C 0.4443(3) 0.4513(10) -0.1182(8) 0.057(3) Uani 0.629(3) 1 d PD A 1
H18 H 0.4519 0.5223 -0.1146 0.068 Uiso 0.629(3) 1 calc PR A 1
C19 C 0.4352(5) 0.4020(13) -0.1962(8) 0.058(3) Uani 0.629(3) 1 d PD A 1
C20 C 0.4243(5) 0.2982(13) -0.1999(8) 0.0528(11) Uani 0.629(3) 1 d PD A 1
H20 H 0.4184 0.2633 -0.2532 0.063 Uiso 0.629(3) 1 calc PR A 1
C21 C 0.4217(6) 0.2441(11) -0.1285(9) 0.0417(10) Uani 0.629(3) 1 d PD A 1
C22 C 0.4536(3) 0.4628(9) 0.0366(7) 0.059(3) Uani 0.629(3) 1 d PD A 1
H22A H 0.4286 0.4672 0.0587 0.089 Uiso 0.629(3) 1 calc PR A 1
H22B H 0.4623 0.5324 0.0247 0.089 Uiso 0.629(3) 1 calc PR A 1
H22C H 0.4771 0.4296 0.0792 0.089 Uiso 0.629(3) 1 calc PR A 1
C23 C 0.4379(7) 0.4584(18) -0.2754(11) 0.085(4) Uani 0.629(3) 1 d PD A 1
H23A H 0.4602 0.4275 -0.2971 0.128 Uiso 0.629(3) 1 calc PR A 1
H23B H 0.4446 0.5312 -0.2617 0.128 Uiso 0.629(3) 1 calc PR A 1
H23C H 0.4105 0.4534 -0.3191 0.128 Uiso 0.629(3) 1 calc PR A 1
C24 C 0.4110(5) 0.1309(12) -0.1426(16) 0.038(3) Uani 0.629(3) 1 d PD A 1
H24A H 0.4317 0.0898 -0.1003 0.057 Uiso 0.629(3) 1 calc PR A 1
H24B H 0.412 0.1111 -0.2001 0.057 Uiso 0.629(3) 1 calc PR A 1
H24C H 0.3824 0.1182 -0.1367 0.057 Uiso 0.629(3) 1 calc PR A 1
C16F C 0.4255(6) 0.2912(18) -0.0520(10) 0.0449(12) Uani 0.371(3) 1 d PD A 2
C17F C 0.4280(7) 0.3992(19) -0.0482(12) 0.050(3) Uani 0.371(3) 1 d PD A 2
C18F C 0.4281(6) 0.4544(19) -0.1205(14) 0.057(3) Uani 0.371(3) 1 d PD A 2
H18F H 0.4303 0.5275 -0.1165 0.068 Uiso 0.371(3) 1 calc PR A 2
C19F C 0.4253(10) 0.409(2) -0.1981(14) 0.058(3) Uani 0.371(3) 1 d PD A 2
C20F C 0.4230(8) 0.302(2) -0.1996(14) 0.0528(11) Uani 0.371(3) 1 d PD A 2
H20F H 0.4214 0.2681 -0.2521 0.063 Uiso 0.371(3) 1 calc PR A 2
C21F C 0.4229(9) 0.2414(19) -0.1296(16) 0.0417(10) Uani 0.371(3) 1 d PD A 2
C22F C 0.4316(5) 0.4585(18) 0.0349(13) 0.059(3) Uani 0.371(3) 1 d PD A 2
H22D H 0.4045 0.4544 0.0495 0.089 Uiso 0.371(3) 1 calc PR A 2
H22E H 0.4384 0.5309 0.0273 0.089 Uiso 0.371(3) 1 calc PR A 2
H22F H 0.4542 0.4279 0.0809 0.089 Uiso 0.371(3) 1 calc PR A 2
C23F C 0.4257(13) 0.471(3) -0.276(2) 0.085(4) Uani 0.371(3) 1 d PD A 2
H23D H 0.3971 0.4979 -0.3028 0.128 Uiso 0.371(3) 1 calc PR A 2
H23E H 0.4344 0.4259 -0.3172 0.128 Uiso 0.371(3) 1 calc PR A 2
H23F H 0.4459 0.5279 -0.2601 0.128 Uiso 0.371(3) 1 calc PR A 2
C24F C 0.4209(11) 0.126(2) -0.140(3) 0.038(3) Uani 0.371(3) 1 d PD A 2
H24D H 0.392 0.1018 -0.1433 0.057 Uiso 0.371(3) 1 calc PR A 2
H24E H 0.4411 0.0934 -0.0908 0.057 Uiso 0.371(3) 1 calc PR A 2
H24F H 0.4282 0.1066 -0.1923 0.057 Uiso 0.371(3) 1 calc PR A 2
C25 C 0.36485(11) -0.0154(3) 0.0990(2) 0.0505(10) Uani 1 1 d . A .
H25A H 0.3399 -0.0204 0.0484 0.061 Uiso 1 1 calc R . .
H25B H 0.3552 -0.0324 0.1499 0.061 Uiso 1 1 calc R . .
C26 C 0.39717(11) -0.0932(3) 0.0907(2) 0.0363(8) Uani 1 1 d . . .
C27 C 0.38582(12) -0.1758(3) 0.0355(2) 0.0509(10) Uani 1 1 d . A .
H27 H 0.3574 -0.1816 0.0004 0.061 Uiso 1 1 calc R . .
C28 C 0.41530(15) -0.2497(3) 0.0306(2) 0.0571(11) Uani 1 1 d . . .
H28 H 0.4069 -0.3062 -0.0074 0.069 Uiso 1 1 calc R A .
C29 C 0.45706(13) -0.2430(3) 0.0804(2) 0.0508(10) Uani 1 1 d . A .
H29 H 0.4773 -0.2943 0.0769 0.061 Uiso 1 1 calc R . .
C30 C 0.46869(11) -0.1602(3) 0.13526(19) 0.0395(9) Uani 1 1 d . . .
H30 H 0.4973 -0.1536 0.1692 0.047 Uiso 1 1 calc R A .
C31 C 0.43895(11) -0.0872(2) 0.14088(19) 0.0354(8) Uani 1 1 d . A .
H31 H 0.4472 -0.0316 0.1799 0.043 Uiso 1 1 calc R . .
O1 O 0.2555(4) 0.5987(12) 0.5099(6) 0.268(9) Uani 0.741(6) 1 d PD B 3
N2 N 0.2977(2) 0.6215(7) 0.4229(4) 0.113(2) Uani 0.741(6) 1 d PD B 3
C32 C 0.3236(4) 0.5431(7) 0.4755(5) 0.188(5) Uani 0.741(6) 1 d PD B 3
H32A H 0.3457 0.5203 0.4493 0.282 Uiso 0.741(6) 1 calc PR B 3
H32B H 0.3056 0.4842 0.4807 0.282 Uiso 0.741(6) 1 calc PR B 3
H32C H 0.337 0.5716 0.5323 0.282 Uiso 0.741(6) 1 calc PR B 3
C33 C 0.3135(3) 0.6648(8) 0.3560(5) 0.158(4) Uani 0.741(6) 1 d PD B 3
H33A H 0.3375 0.6232 0.3494 0.237 Uiso 0.741(6) 1 calc PR B 3
H33B H 0.3231 0.7358 0.3709 0.237 Uiso 0.741(6) 1 calc PR B 3
H33C H 0.2908 0.6647 0.3023 0.237 Uiso 0.741(6) 1 calc PR B 3
C34 C 0.2654(3) 0.6484(9) 0.4551(6) 0.219(9) Uani 0.741(6) 1 d PD B 3
H34 H 0.2497 0.709 0.434 0.262 Uiso 0.741(6) 1 calc PR B 3
O1F O 0.2585(11) 0.523(4) 0.527(2) 0.268(9) Uani 0.259(6) 1 d PD B 4
N2F N 0.2979(6) 0.5358(16) 0.4337(11) 0.113(2) Uani 0.259(6) 1 d PD B 4
C32F C 0.3251(10) 0.4563(18) 0.4865(13) 0.188(5) Uani 0.259(6) 1 d PD B 4
H32D H 0.3509 0.4473 0.4679 0.282 Uiso 0.259(6) 1 calc PR B 4
H32E H 0.3095 0.3908 0.4803 0.282 Uiso 0.259(6) 1 calc PR B 4
H32F H 0.3328 0.4778 0.5465 0.282 Uiso 0.259(6) 1 calc PR B 4
C33F C 0.3104(8) 0.560(2) 0.3559(12) 0.158(4) Uani 0.259(6) 1 d PD B 4
H33D H 0.3387 0.5315 0.3605 0.237 Uiso 0.259(6) 1 calc PR B 4
H33E H 0.3111 0.6352 0.349 0.237 Uiso 0.259(6) 1 calc PR B 4
H33F H 0.2898 0.5299 0.3064 0.237 Uiso 0.259(6) 1 calc PR B 4
C34F C 0.2633(7) 0.559(3) 0.4617(17) 0.219(9) Uani 0.259(6) 1 d PD B 4
H34F H 0.2424 0.6051 0.4292 0.262 Uiso 0.259(6) 1 calc PR B 4



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

_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 C6 1.841(4) 2_655 ?
P1 C7 1.860(6) . ?
P1 C1 1.860(3) . ?
P1 C7F 1.884(10) . ?
P2 C3 1.833(3) . ?
P2 C16F 1.841(12) . ?
P2 C2 1.844(3) . ?
P2 C16 1.859(8) . ?
N1 C25 1.458(4) . ?
N1 C2 1.465(4) . ?
N1 C1 1.475(4) . ?
C3 C4 1.511(4) . ?
C4 C5 1.522(5) . ?
C5 C6 1.517(4) . ?
C6 P1 1.841(4) 2_655 ?
C7 C8 1.397(8) . ?
C7 C12 1.407(8) . ?
C8 C9 1.391(8) . ?
C8 C13 1.516(8) . ?
C9 C10 1.382(8) . ?
C10 C11 1.361(8) . ?
C10 C14 1.531(8) . ?
C11 C12 1.385(7) . ?
C12 C15 1.509(9) . ?
C7F C12F 1.395(11) . ?
C7F C8F 1.399(12) . ?
C8F C9F 1.394(12) . ?
C8F C13F 1.485(14) . ?
C9F C10F 1.383(12) . ?
C10F C11F 1.392(11) . ?
C10F C14F 1.542(12) . ?
C11F C12F 1.390(11) . ?
C12F C15F 1.507(13) . ?
C16 C21 1.408(8) . ?
C16 C17 1.410(8) . ?
C17 C18 1.379(8) . ?
C17 C22 1.528(8) . ?
C18 C19 1.380(8) . ?
C19 C20 1.388(8) . ?
C19 C23 1.507(8) . ?
C20 C21 1.382(8) . ?
C21 C24 1.511(8) . ?
C16F C21F 1.401(12) . ?
C16F C17F 1.402(12) . ?
C17F C18F 1.378(12) . ?
C17F C22F 1.533(13) . ?
C18F C19F 1.375(12) . ?
C19F C20F 1.386(12) . ?
C19F C23F 1.509(13) . ?
C20F C21F 1.386(12) . ?
C21F C24F 1.508(13) . ?
C25 C26 1.492(5) . ?
C26 C27 1.381(5) . ?
C26 C31 1.386(4) . ?
C27 C28 1.375(5) . ?
C28 C29 1.384(5) . ?
C29 C30 1.380(4) . ?
C30 C31 1.377(4) . ?
O1 C34 1.215(5) . ?
N2 C34 1.346(5) . ?
N2 C33 1.441(5) . ?
N2 C32 1.443(5) . ?
O1F C34F 1.208(5) . ?
N2F C34F 1.365(5) . ?
N2F C33F 1.468(5) . ?
N2F C32F 1.472(5) . ?

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
C6 P1 C7 97.6(2) 2_655 . ?
C6 P1 C1 101.05(18) 2_655 . ?
C7 P1 C1 105.1(2) . . ?
C6 P1 C7F 118.4(4) 2_655 . ?
C7 P1 C7F 22.0(4) . . ?
C1 P1 C7F 105.3(4) . . ?
C3 P2 C16F 104.1(6) . . ?
C3 P2 C2 99.64(15) . . ?
C16F P2 C2 105.2(8) . . ?
C3 P2 C16 100.8(3) . . ?
C16F P2 C16 4.7(10) . . ?
C2 P2 C16 109.2(5) . . ?
C25 N1 C2 111.3(3) . . ?
C25 N1 C1 110.7(3) . . ?
C2 N1 C1 111.6(3) . . ?
N1 C1 P1 106.3(2) . . ?
N1 C2 P2 108.0(2) . . ?
C4 C3 P2 114.3(2) . . ?
C3 C4 C5 111.8(3) . . ?
C6 C5 C4 113.8(3) . . ?
C5 C6 P1 110.3(3) . 2_655 ?
C8 C7 C12 118.6(6) . . ?
C8 C7 P1 111.2(5) . . ?
C12 C7 P1 130.2(5) . . ?
C9 C8 C7 120.1(6) . . ?
C9 C8 C13 117.6(8) . . ?
C7 C8 C13 122.1(7) . . ?
C10 C9 C8 121.0(6) . . ?
C11 C10 C9 118.5(6) . . ?
C11 C10 C14 121.2(7) . . ?
C9 C10 C14 120.3(7) . . ?
C10 C11 C12 122.8(7) . . ?
C11 C12 C7 119.0(6) . . ?
C11 C12 C15 117.2(6) . . ?
C7 C12 C15 123.8(6) . . ?
C12F C7F C8F 118.7(10) . . ?
C12F C7F P1 118.5(8) . . ?
C8F C7F P1 122.2(8) . . ?
C9F C8F C7F 120.8(12) . . ?
C9F C8F C13F 115.6(15) . . ?
C7F C8F C13F 123.6(14) . . ?
C10F C9F C8F 120.3(11) . . ?
C9F C10F C11F 118.9(10) . . ?
C9F C10F C14F 120.8(11) . . ?
C11F C10F C14F 120.3(11) . . ?
C12F C11F C10F 121.4(10) . . ?
C11F C12F C7F 119.9(10) . . ?
C11F C12F C15F 115.4(10) . . ?
C7F C12F C15F 124.7(9) . . ?
C21 C16 C17 117.9(6) . . ?
C21 C16 P2 125.2(9) . . ?
C17 C16 P2 116.9(8) . . ?
C18 C17 C16 120.9(6) . . ?
C18 C17 C22 115.7(8) . . ?
C16 C17 C22 123.4(9) . . ?
C17 C18 C19 121.0(7) . . ?
C18 C19 C20 118.5(7) . . ?
C18 C19 C23 121.0(10) . . ?
C20 C19 C23 120.5(10) . . ?
C21 C20 C19 121.9(7) . . ?
C20 C21 C16 119.8(7) . . ?
C20 C21 C24 115.3(9) . . ?
C16 C21 C24 124.9(10) . . ?
C21F C16F C17F 119.2(11) . . ?
C21F C16F P2 129.3(15) . . ?
C17F C16F P2 111.5(14) . . ?
C18F C17F C16F 119.6(12) . . ?
C18F C17F C22F 118.5(15) . . ?
C16F C17F C22F 121.9(15) . . ?
C19F C18F C17F 123.2(13) . . ?
C18F C19F C20F 115.8(12) . . ?
C18F C19F C23F 122.5(17) . . ?
C20F C19F C23F 121.8(17) . . ?
C21F C20F C19F 124.3(13) . . ?
C20F C21F C16F 117.9(12) . . ?
C20F C21F C24F 118.8(16) . . ?
C16F C21F C24F 123.3(16) . . ?
N1 C25 C26 113.8(3) . . ?
C27 C26 C31 118.1(3) . . ?
C27 C26 C25 120.8(3) . . ?
C31 C26 C25 121.0(3) . . ?
C28 C27 C26 120.6(3) . . ?
C27 C28 C29 121.0(3) . . ?
C30 C29 C28 118.6(4) . . ?
C31 C30 C29 120.2(3) . . ?
C30 C31 C26 121.4(3) . . ?
C34 N2 C33 132.6(7) . . ?
C34 N2 C32 110.1(7) . . ?
C33 N2 C32 116.8(5) . . ?
O1 C34 N2 123.1(7) . . ?
C34F N2F C33F 133.9(18) . . ?
C34F N2F C32F 112.3(18) . . ?
C33F N2F C32F 113.0(6) . . ?
O1F C34F N2F 121.9(8) . . ?



#------------------------------------------------------------------------------#
#                            END OF DATA BLOCK                                 #
#------------------------------------------------------------------------------#


_database_code_depnum_ccdc_archive 'CCDC 973340'
#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
(RSSR)-1,11-dibenzyl-3,9,13,19-tetramesityl-1,11-diaza-3,9,13,19-tetraphosphacycloeicosane
_chemical_name_common            ?
_chemical_formula_moiety         'C64 H86 N2 P4'
_chemical_formula_sum            'C64 H86 N2 P4'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless

_diffrn_ambient_temperature      296(2)
_chemical_formula_weight         1007.22

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.978(7)
_cell_length_b                   11.999(9)
_cell_length_c                   15.378(11)
_cell_angle_alpha                77.012(8)
_cell_angle_beta                 86.156(9)
_cell_angle_gamma                70.547(8)
_cell_volume                     1522.2(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1868
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      20.66
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_F_000             544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.162
_shelx_estimated_absorpt_T_min   0.953
_shelx_estimated_absorpt_T_max   0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              SmartApex2
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11374
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.041
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             5840
_reflns_number_gt                3124
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX - Version 1.80.05 (Farrugia, 1999)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1402P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5840
_refine_ls_number_parameters     322
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_gt           0.0778
_refine_ls_wR_factor_ref         0.2573
_refine_ls_wR_factor_gt          0.2112
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.014
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P2 P 1.00594(12) 0.05483(9) 0.24619(7) 0.0547(3) Uani 1 1 d . . . . .
P1 P 0.48817(13) 0.14791(9) -0.19525(7) 0.0590(4) Uani 1 1 d . . . . .
N1 N 1.3024(4) 0.0650(3) 0.2234(2) 0.0546(8) Uani 1 1 d . . . . .
C4 C 0.6717(5) 0.1287(4) -0.0486(2) 0.0595(10) Uani 1 1 d . . . . .
H4A H 0.5752 0.1505 -0.0147 0.071 Uiso 1 1 calc R U . . .
H4B H 0.7062 0.0419 -0.0439 0.071 Uiso 1 1 calc R U . . .
C7 C 0.9634(5) 0.1265(4) 0.1285(2) 0.0572(10) Uani 1 1 d . . . . .
H7A H 0.9411 0.2130 0.1211 0.069 Uiso 1 1 calc R U . . .
H7B H 1.0570 0.0962 0.0941 0.069 Uiso 1 1 calc R U . . .
C6 C 0.8268(5) 0.1057(4) 0.0907(2) 0.0594(10) Uani 1 1 d . . . . .
H6A H 0.7322 0.1396 0.1232 0.071 Uiso 1 1 calc R U . . .
H6B H 0.8467 0.0193 0.1007 0.071 Uiso 1 1 calc R U . . .
C8 C 0.3716(5) 0.2865(3) -0.2737(2) 0.0552(10) Uani 1 1 d . . . . .
C5 C 0.7961(5) 0.1601(4) -0.0081(2) 0.0610(11) Uani 1 1 d . . . . .
H5A H 0.7648 0.2475 -0.0171 0.073 Uiso 1 1 calc R U . . .
H5B H 0.8941 0.1333 -0.0399 0.073 Uiso 1 1 calc R U . . .
C2 C 1.1552(4) 0.1189(3) 0.2690(3) 0.0573(10) Uani 1 1 d . . . . .
H2A H 1.1178 0.2060 0.2477 0.069 Uiso 1 1 calc R U . . .
H2B H 1.1742 0.1014 0.3328 0.069 Uiso 1 1 calc R U . . .
C3 C 0.6368(5) 0.1920(4) -0.1457(3) 0.0660(11) Uani 1 1 d . . . . .
H3A H 0.7339 0.1724 -0.1794 0.079 Uiso 1 1 calc R U . . .
H3B H 0.5986 0.2788 -0.1503 0.079 Uiso 1 1 calc R U . . .
C17 C 0.8362(4) 0.1251(4) 0.3134(2) 0.0548(10) Uani 1 1 d . . . . .
C18 C 0.7350(5) 0.2455(4) 0.2940(3) 0.0587(10) Uani 1 1 d . . . . .
C9 C 0.4359(5) 0.3658(4) -0.3355(3) 0.0650(11) Uani 1 1 d . . . . .
C22 C 0.8041(5) 0.0463(4) 0.3889(3) 0.0645(11) Uani 1 1 d . . . . .
C11 C 0.1731(7) 0.4974(4) -0.3846(3) 0.0801(14) Uani 1 1 d . . . . .
C10 C 0.3321(6) 0.4683(4) -0.3890(3) 0.0721(13) Uani 1 1 d . . . . .
H10 H 0.3743 0.5194 -0.4300 0.086 Uiso 1 1 calc R U . . .
C27 C 1.3315(5) 0.2588(4) 0.1423(3) 0.0722(13) Uani 1 1 d . . . . .
C1 C 1.3897(5) -0.0570(3) 0.2730(3) 0.0623(11) Uani 1 1 d . . . . .
H1A H 1.3160 -0.0959 0.3033 0.075 Uiso 1 1 calc R U . . .
H1B H 1.4570 -0.0518 0.3176 0.075 Uiso 1 1 calc R U . . .
C13 C 0.2073(5) 0.3146(4) -0.2690(3) 0.0673(11) Uani 1 1 d . . . . .
C21 C 0.6710(5) 0.0862(4) 0.4397(3) 0.0716(12) Uani 1 1 d . . . . .
H21 H 0.6519 0.0327 0.4896 0.086 Uiso 1 1 calc R U . . .
C19 C 0.6023(5) 0.2801(4) 0.3470(3) 0.0638(11) Uani 1 1 d . . . . .
H19 H 0.5347 0.3596 0.3331 0.077 Uiso 1 1 calc R U . . .
C23 C 0.7592(6) 0.3436(4) 0.2187(3) 0.0815(14) Uani 1 1 d . . . . .
H23A H 0.7216 0.3370 0.1637 0.122 Uiso 1 1 calc R U . . .
H23B H 0.8696 0.3344 0.2137 0.122 Uiso 1 1 calc R U . . .
H23C H 0.7017 0.4216 0.2310 0.122 Uiso 1 1 calc R U . . .
C12 C 0.1112(6) 0.4194(4) -0.3252(4) 0.0822(14) Uani 1 1 d . . . . .
H12 H 0.0022 0.4372 -0.3224 0.099 Uiso 1 1 calc R U . . .
C26 C 1.4029(5) 0.1416(4) 0.2070(3) 0.0759(13) Uani 1 1 d . . . . .
H26A H 1.5035 0.0978 0.1840 0.091 Uiso 1 1 calc R U . . .
H26B H 1.4231 0.1583 0.2631 0.091 Uiso 1 1 calc R U . . .
C20 C 0.5672(5) 0.2017(4) 0.4188(3) 0.0688(12) Uani 1 1 d . . . . .
C16 C 0.1273(6) 0.2355(5) -0.2085(4) 0.0953(17) Uani 1 1 d . . . . .
H16A H 0.1572 0.1582 -0.2246 0.143 Uiso 1 1 calc R U . . .
H16B H 0.0148 0.2731 -0.2143 0.143 Uiso 1 1 calc R U . . .
H16C H 0.1585 0.2246 -0.1479 0.143 Uiso 1 1 calc R U . . .
C28 C 1.2893(6) 0.2637(4) 0.0575(4) 0.0826(14) Uani 1 1 d . U . . .
H28 H 1.3020 0.1919 0.0399 0.099 Uiso 1 1 calc R U . . .
C15 C 0.0641(7) 0.6136(5) -0.4423(4) 0.114(2) Uani 1 1 d . . . . .
H15A H 0.0660 0.6821 -0.4205 0.172 Uiso 1 1 calc R U . . .
H15B H -0.0418 0.6108 -0.4397 0.172 Uiso 1 1 calc R U . . .
H15C H 0.0996 0.6209 -0.5030 0.172 Uiso 1 1 calc R U . . .
C14 C 0.6081(6) 0.3463(5) -0.3492(4) 0.0927(16) Uani 1 1 d . . . . .
H14A H 0.6232 0.4213 -0.3782 0.139 Uiso 1 1 calc R U . . .
H14B H 0.6504 0.2878 -0.3856 0.139 Uiso 1 1 calc R U . . .
H14C H 0.6616 0.3171 -0.2924 0.139 Uiso 1 1 calc R U . . .
C25 C 0.9139(6) -0.0842(4) 0.4211(3) 0.0923(17) Uani 1 1 d . . . . .
H25A H 0.8777 -0.1191 0.4774 0.138 Uiso 1 1 calc R U . . .
H25B H 1.0194 -0.0842 0.4278 0.138 Uiso 1 1 calc R U . . .
H25C H 0.9131 -0.1310 0.3781 0.138 Uiso 1 1 calc R U . . .
C24 C 0.4158(6) 0.2390(5) 0.4709(4) 0.0980(17) Uani 1 1 d . . . . .
H24A H 0.3939 0.3205 0.4779 0.147 Uiso 1 1 calc R U . . .
H24B H 0.4277 0.1857 0.5287 0.147 Uiso 1 1 calc R U . . .
H24C H 0.3301 0.2345 0.4393 0.147 Uiso 1 1 calc R U . . .
C32 C 1.3061(7) 0.3671(5) 0.1670(4) 0.1087(19) Uani 1 1 d . U . . .
H32 H 1.3309 0.3667 0.2248 0.130 Uiso 1 1 calc R U . . .
C29 C 1.2285(7) 0.3719(6) -0.0027(4) 0.113(2) Uani 1 1 d . U . . .
H29 H 1.2035 0.3724 -0.0605 0.136 Uiso 1 1 calc R U . . .
C30 C 1.2052(9) 0.4787(6) 0.0226(5) 0.131(2) Uani 1 1 d . U . . .
H30 H 1.1630 0.5520 -0.0176 0.157 Uiso 1 1 calc R U . . .
C31 C 1.2441(9) 0.4768(5) 0.1070(6) 0.136(2) Uani 1 1 d . U . . .
H31 H 1.2292 0.5490 0.1246 0.163 Uiso 1 1 calc R U . . .


_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
P2 C7 1.827(4) . ?
P2 C2 1.839(4) . ?
P2 C17 1.851(4) . ?
P1 C8 1.851(4) . ?
P1 C3 1.852(4) . ?
P1 C1 1.853(4) 2_755 ?
N1 C26 1.463(5) . ?
N1 C1 1.467(4) . ?
N1 C2 1.472(5) . ?
C4 C5 1.501(5) . ?
C4 C3 1.517(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 C6 1.506(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C6 C5 1.517(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C8 C13 1.399(5) . ?
C8 C9 1.424(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C17 C22 1.403(5) . ?
C17 C18 1.404(5) . ?
C18 C19 1.396(5) . ?
C18 C23 1.515(5) . ?
C9 C10 1.394(5) . ?
C9 C14 1.492(6) . ?
C22 C21 1.389(6) . ?
C22 C25 1.536(6) . ?
C11 C10 1.353(6) . ?
C11 C12 1.383(7) . ?
C11 C15 1.530(6) . ?
C10 H10 0.9300 . ?
C27 C28 1.365(7) . ?
C27 C32 1.377(7) . ?
C27 C26 1.495(6) . ?
C1 P1 1.853(4) 2_755 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C13 C12 1.400(6) . ?
C13 C16 1.500(6) . ?
C21 C20 1.368(6) . ?
C21 H21 0.9300 . ?
C19 C20 1.373(6) . ?
C19 H19 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C12 H12 0.9300 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C20 C24 1.517(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C28 C29 1.377(7) . ?
C28 H28 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C32 C31 1.389(7) . ?
C32 H32 0.9300 . ?
C29 C30 1.367(9) . ?
C29 H29 0.9300 . ?
C30 C31 1.360(10) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 P2 C2 100.58(17) . . ?
C7 P2 C17 108.84(18) . . ?
C2 P2 C17 102.62(19) . . ?
C8 P1 C3 105.25(19) . . ?
C8 P1 C1 101.59(18) . 2_755 ?
C3 P1 C1 101.7(2) . 2_755 ?
C26 N1 C1 110.7(3) . . ?
C26 N1 C2 112.2(3) . . ?
C1 N1 C2 111.3(3) . . ?
C5 C4 C3 113.2(3) . . ?
C5 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.8 . . ?
C6 C7 P2 114.4(3) . . ?
C6 C7 H7A 108.7 . . ?
P2 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
P2 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C7 C6 C5 114.6(3) . . ?
C7 C6 H6A 108.6 . . ?
C5 C6 H6A 108.6 . . ?
C7 C6 H6B 108.6 . . ?
C5 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
C13 C8 C9 118.9(4) . . ?
C13 C8 P1 115.9(3) . . ?
C9 C8 P1 125.2(3) . . ?
C4 C5 C6 115.0(3) . . ?
C4 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
C4 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
N1 C2 P2 108.8(3) . . ?
N1 C2 H2A 109.9 . . ?
P2 C2 H2A 109.9 . . ?
N1 C2 H2B 109.9 . . ?
P2 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
C4 C3 P1 112.4(3) . . ?
C4 C3 H3A 109.1 . . ?
P1 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
P1 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C22 C17 C18 118.1(4) . . ?
C22 C17 P2 115.1(3) . . ?
C18 C17 P2 126.7(3) . . ?
C19 C18 C17 119.0(4) . . ?
C19 C18 C23 116.4(4) . . ?
C17 C18 C23 124.6(4) . . ?
C10 C9 C8 118.4(4) . . ?
C10 C9 C14 116.8(4) . . ?
C8 C9 C14 124.8(4) . . ?
C21 C22 C17 120.2(4) . . ?
C21 C22 C25 117.1(4) . . ?
C17 C22 C25 122.7(4) . . ?
C10 C11 C12 117.9(4) . . ?
C10 C11 C15 121.4(5) . . ?
C12 C11 C15 120.7(5) . . ?
C11 C10 C9 123.5(4) . . ?
C11 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
C28 C27 C32 117.4(4) . . ?
C28 C27 C26 122.2(5) . . ?
C32 C27 C26 120.3(5) . . ?
N1 C1 P1 109.9(3) . 2_755 ?
N1 C1 H1A 109.7 . . ?
P1 C1 H1A 109.7 2_755 . ?
N1 C1 H1B 109.7 . . ?
P1 C1 H1B 109.7 2_755 . ?
H1A C1 H1B 108.2 . . ?
C8 C13 C12 119.2(4) . . ?
C8 C13 C16 123.3(4) . . ?
C12 C13 C16 117.5(4) . . ?
C20 C21 C22 122.1(4) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C20 C19 C18 122.9(4) . . ?
C20 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C11 C12 C13 122.2(5) . . ?
C11 C12 H12 118.9 . . ?
C13 C12 H12 118.9 . . ?
N1 C26 C27 113.1(3) . . ?
N1 C26 H26A 109.0 . . ?
C27 C26 H26A 109.0 . . ?
N1 C26 H26B 109.0 . . ?
C27 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
C21 C20 C19 117.5(4) . . ?
C21 C20 C24 120.7(4) . . ?
C19 C20 C24 121.7(5) . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C27 C28 C29 121.9(5) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C20 C24 H24A 109.5 . . ?
C20 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C20 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C27 C32 C31 121.1(6) . . ?
C27 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C30 C29 C28 119.9(6) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C31 C30 C29 119.5(6) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C30 C31 C32 120.0(6) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?

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
C2 P2 C7 C6 -172.2(3) . . . . ?
C17 P2 C7 C6 -64.9(3) . . . . ?
P2 C7 C6 C5 -177.2(3) . . . . ?
C3 P1 C8 C13 -133.6(3) . . . . ?
C1 P1 C8 C13 120.7(3) 2_755 . . . ?
C3 P1 C8 C9 45.1(4) . . . . ?
C1 P1 C8 C9 -60.6(4) 2_755 . . . ?
C3 C4 C5 C6 176.0(3) . . . . ?
C7 C6 C5 C4 173.7(3) . . . . ?
C26 N1 C2 P2 156.8(3) . . . . ?
C1 N1 C2 P2 -78.5(3) . . . . ?
C7 P2 C2 N1 -71.0(3) . . . . ?
C17 P2 C2 N1 176.8(2) . . . . ?
C5 C4 C3 P1 178.1(3) . . . . ?
C8 P1 C3 C4 144.5(3) . . . . ?
C1 P1 C3 C4 -109.9(3) 2_755 . . . ?
C7 P2 C17 C22 145.2(3) . . . . ?
C2 P2 C17 C22 -108.8(3) . . . . ?
C7 P2 C17 C18 -31.8(4) . . . . ?
C2 P2 C17 C18 74.1(4) . . . . ?
C22 C17 C18 C19 -3.8(6) . . . . ?
P2 C17 C18 C19 173.2(3) . . . . ?
C22 C17 C18 C23 175.8(4) . . . . ?
P2 C17 C18 C23 -7.2(6) . . . . ?
C13 C8 C9 C10 -0.1(6) . . . . ?
P1 C8 C9 C10 -178.7(3) . . . . ?
C13 C8 C9 C14 -178.7(4) . . . . ?
P1 C8 C9 C14 2.7(7) . . . . ?
C18 C17 C22 C21 3.2(6) . . . . ?
P2 C17 C22 C21 -174.1(3) . . . . ?
C18 C17 C22 C25 -174.9(4) . . . . ?
P2 C17 C22 C25 7.8(6) . . . . ?
C12 C11 C10 C9 -1.6(7) . . . . ?
C15 C11 C10 C9 177.6(5) . . . . ?
C8 C9 C10 C11 0.9(7) . . . . ?
C14 C9 C10 C11 179.6(5) . . . . ?
C26 N1 C1 P1 -81.6(4) . . . 2_755 ?
C2 N1 C1 P1 152.9(3) . . . 2_755 ?
C9 C8 C13 C12 0.0(6) . . . . ?
P1 C8 C13 C12 178.8(3) . . . . ?
C9 C8 C13 C16 178.0(4) . . . . ?
P1 C8 C13 C16 -3.3(6) . . . . ?
C17 C22 C21 C20 0.1(7) . . . . ?
C25 C22 C21 C20 178.3(4) . . . . ?
C17 C18 C19 C20 1.2(6) . . . . ?
C23 C18 C19 C20 -178.4(4) . . . . ?
C10 C11 C12 C13 1.5(8) . . . . ?
C15 C11 C12 C13 -177.6(5) . . . . ?
C8 C13 C12 C11 -0.8(8) . . . . ?
C16 C13 C12 C11 -178.9(5) . . . . ?
C1 N1 C26 C27 169.0(4) . . . . ?
C2 N1 C26 C27 -66.0(5) . . . . ?
C28 C27 C26 N1 -58.2(6) . . . . ?
C32 C27 C26 N1 121.9(5) . . . . ?
C22 C21 C20 C19 -2.7(7) . . . . ?
C22 C21 C20 C24 174.7(4) . . . . ?
C18 C19 C20 C21 2.1(7) . . . . ?
C18 C19 C20 C24 -175.3(4) . . . . ?
C32 C27 C28 C29 2.1(8) . . . . ?
C26 C27 C28 C29 -177.7(5) . . . . ?
C28 C27 C32 C31 -1.7(8) . . . . ?
C26 C27 C32 C31 178.1(5) . . . . ?
C27 C28 C29 C30 -1.7(9) . . . . ?
C28 C29 C30 C31 0.8(11) . . . . ?
C29 C30 C31 C32 -0.4(12) . . . . ?
C27 C32 C31 C30 0.9(11) . . . . ?

_refine_diff_density_max         0.526
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.080

_shelxl_version_number           2013-3

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?

_database_code_depnum_ccdc_archive 'CCDC 974210'
