# 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
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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#
data_I
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H59 I O4 P2 Pd'
_chemical_formula_iupac          ?
_chemical_formula_weight         1091.27
_chemical_absolute_configuration ad

_chemical_melting_point          ?

_space_group_crystal_system      hexagonal
_space_group_name_H-M_alt        'P 65'
_space_group_name_Hall           'P 65'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'

_cell_length_a                   13.4441(2)
_cell_length_b                   13.4441(2)
_cell_length_c                   49.8415(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7801.6(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9423
_cell_measurement_theta_min      2.6899
_cell_measurement_theta_max      26.1007
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3336

_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_T_max  0.85

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            45660
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.964
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_limit_l_max       47

_refine_special_details          
;
;

_reflns_number_total             9461
_reflns_number_gt                9141
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0553
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.087
_refine_ls_number_reflns         9461
_refine_ls_number_parameters     673
_refine_ls_number_restraints     411
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0199P)²+4.0172P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.388
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Flack x determined using 3960 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.004(6)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd1 0.30324(3) 0.69677(3) 0.50027(2) 0.01418(7) Uani d . . . 1.0 . .
C C1 0.2156(3) 0.7841(3) 0.50020(12) 0.0148(8) Uani d . . . 1.0 . .
C C2 0.1514(3) 0.7821(4) 0.52277(10) 0.0166(10) Uani d . . . 1.0 . .
C C3 0.0944(4) 0.8447(4) 0.52270(11) 0.0213(11) Uani d . . . 1.0 . .
H H3 0.0549 0.8462 0.5384 0.026 Uiso calc U . R 1.0 . .
C C4 0.0945(4) 0.9049(4) 0.50008(15) 0.0272(11) Uani d . . . 1.0 . .
H H4 0.0531 0.9451 0.5 0.033 Uiso calc U . R 1.0 . .
C C5 0.1551(4) 0.9059(4) 0.47776(11) 0.0210(11) Uani d . . . 1.0 . .
H H5 0.1542 0.9461 0.4622 0.025 Uiso calc U . R 1.0 . .
C C6 0.2180(4) 0.8486(3) 0.47764(10) 0.0168(10) Uani d . . . 1.0 . .
C C7 0.2960(4) 0.8630(4) 0.45472(10) 0.0176(10) Uani d . . . 1.0 . .
H H7 0.262 0.8691 0.4374 0.021 Uiso calc U . R 1.0 . .
C C8 0.4167(4) 0.9690(3) 0.45885(11) 0.0216(11) Uani d . . . 1.0 . .
H H8A 0.4539 0.9571 0.4747 0.026 Uiso calc U . R 1.0 . .
H H8B 0.4652 0.9798 0.4429 0.026 Uiso calc U . R 1.0 . .
C C9 0.4054(4) 1.0751(4) 0.46300(11) 0.0225(11) Uani d . . . 1.0 . .
C C10 0.4335(4) 1.1342(4) 0.48946(10) 0.0191(11) Uani d . . . 1.0 . .
C C11 0.4368(5) 1.2392(4) 0.49158(11) 0.0304(13) Uani d . . . 1.0 . .
H H11 0.4239 1.2725 0.4761 0.036 Uiso calc U . R 1.0 . .
C C12 0.4585(5) 1.2951(4) 0.51575(13) 0.0360(14) Uani d . . . 1.0 . .
H H12 0.4611 1.3669 0.5169 0.043 Uiso calc U . R 1.0 . .
C C13 0.4766(5) 1.2476(4) 0.53853(13) 0.0322(14) Uani d . . . 1.0 . .
H H13 0.491 1.2857 0.5553 0.039 Uiso calc U . R 1.0 . .
C C14 0.4736(5) 1.1437(4) 0.53638(12) 0.0353(14) Uani d . . . 1.0 . .
H H14 0.4868 1.1109 0.5519 0.042 Uiso calc U . R 1.0 . .
C C15 0.4518(4) 1.0869(4) 0.51231(11) 0.0281(12) Uani d . . . 1.0 . .
H H15 0.4492 1.0151 0.5113 0.034 Uiso calc U . R 1.0 . .
C C16 0.4301(4) 0.7652(4) 0.43358(10) 0.0177(11) Uani d . . . 1.0 . .
C C17 0.4184(4) 0.7509(4) 0.40603(12) 0.0258(12) Uani d . . . 1.0 . .
H H17 0.3442 0.7161 0.3981 0.031 Uiso calc U . R 1.0 . .
C C18 0.5156(5) 0.7875(4) 0.38980(13) 0.0330(14) Uani d . . . 1.0 . .
H H18 0.5076 0.7764 0.3709 0.04 Uiso calc U . R 1.0 . .
C C19 0.6235(4) 0.8402(4) 0.40149(13) 0.0339(15) Uani d . . . 1.0 . .
H H19 0.6897 0.8667 0.3905 0.041 Uiso calc U . R 1.0 . .
C C20 0.6358(5) 0.8545(4) 0.42890(13) 0.0336(14) Uani d . . . 1.0 . .
H H20 0.7102 0.8907 0.4367 0.04 Uiso calc U . R 1.0 . .
C C21 0.5391(4) 0.8158(4) 0.44509(13) 0.0266(13) Uani d . . . 1.0 . .
H H21 0.5474 0.824 0.464 0.032 Uiso calc U . R 1.0 . .
C C22 0.1828(4) 0.6198(4) 0.43795(10) 0.0164(10) Uani d . . . 1.0 . .
C C23 0.1251(4) 0.6429(4) 0.41767(10) 0.0197(10) Uani d . . . 1.0 . .
H H23 0.1491 0.7201 0.4129 0.024 Uiso calc U . R 1.0 . .
C C24 0.0330(4) 0.5533(4) 0.40459(10) 0.0211(11) Uani d . . . 1.0 . .
H H24 -0.0046 0.5692 0.3905 0.025 Uiso calc U . R 1.0 . .
C C25 -0.0045(4) 0.4411(4) 0.41189(11) 0.0233(11) Uani d . . . 1.0 . .
H H25 -0.0683 0.3801 0.403 0.028 Uiso calc U . R 1.0 . .
C C26 0.0508(4) 0.4170(4) 0.43222(11) 0.0241(11) Uani d . . . 1.0 . .
H H26 0.025 0.3396 0.4372 0.029 Uiso calc U . R 1.0 . .
C C27 0.1438(4) 0.5060(4) 0.44533(10) 0.0198(11) Uani d . . . 1.0 . .
H H27 0.181 0.4895 0.4594 0.024 Uiso calc U . R 1.0 . .
C C28 0.1375(4) 0.7040(4) 0.54600(10) 0.0164(10) Uani d . . . 1.0 . .
H H28 0.1315 0.7381 0.5633 0.02 Uiso calc U . R 1.0 . .
C C29 0.0312(3) 0.5831(4) 0.54172(10) 0.0214(11) Uani d . . . 1.0 . .
H H29A 0.0433 0.5462 0.5258 0.026 Uiso calc U . R 1.0 . .
H H29B 0.0203 0.5342 0.5576 0.026 Uiso calc U . R 1.0 . .
C C30 -0.0755(4) 0.5943(4) 0.53757(11) 0.0222(11) Uani d . . . 1.0 . .
C C31 -0.1341(4) 0.5665(4) 0.51116(10) 0.0192(11) Uani d . . . 1.0 . .
C C32 -0.2385(4) 0.5634(5) 0.50892(11) 0.0323(14) Uani d . . . 1.0 . .
H H32 -0.2717 0.5762 0.5244 0.039 Uiso calc U . R 1.0 . .
C C33 -0.2948(4) 0.5422(5) 0.48485(13) 0.0363(14) Uani d . . . 1.0 . .
H H33 -0.366 0.541 0.4837 0.044 Uiso calc U . R 1.0 . .
C C34 -0.2478(5) 0.5229(5) 0.46227(13) 0.0332(14) Uani d . . . 1.0 . .
H H34 -0.2869 0.5069 0.4456 0.04 Uiso calc U . R 1.0 . .
C C35 -0.1433(4) 0.5269(5) 0.46417(12) 0.0355(14) Uani d . . . 1.0 . .
H H35 -0.1103 0.5147 0.4485 0.043 Uiso calc U . R 1.0 . .
C C36 -0.0864(4) 0.5481(4) 0.48824(11) 0.0284(12) Uani d . . . 1.0 . .
H H36 -0.0148 0.5501 0.4892 0.034 Uiso calc U . R 1.0 . .
C C37 0.3799(4) 0.8170(4) 0.56258(10) 0.0171(10) Uani d . . . 1.0 . .
C C38 0.4936(4) 0.8561(4) 0.55516(10) 0.0201(10) Uani d . . . 1.0 . .
H H38 0.5101 0.8188 0.5411 0.024 Uiso calc U . R 1.0 . .
C C39 0.5828(4) 0.9493(4) 0.56826(11) 0.0246(11) Uani d . . . 1.0 . .
H H39 0.6601 0.9751 0.5632 0.03 Uiso calc U . R 1.0 . .
C C40 0.5594(4) 1.0048(4) 0.58861(11) 0.0237(12) Uani d . . . 1.0 . .
H H40 0.6205 1.0686 0.5975 0.028 Uiso calc U . R 1.0 . .
C C41 0.4469(4) 0.9670(4) 0.59595(11) 0.0214(11) Uani d . . . 1.0 . .
H H41 0.4311 1.0046 0.61 0.026 Uiso calc U . R 1.0 . .
C C42 0.3570(4) 0.8748(4) 0.58295(10) 0.0197(10) Uani d . . . 1.0 . .
H H42 0.2799 0.8506 0.5878 0.024 Uiso calc U . R 1.0 . .
C C43 0.2346(4) 0.5700(4) 0.56684(11) 0.0198(11) Uani d . . . 1.0 . .
C C44 0.2498(4) 0.5818(4) 0.59445(12) 0.0260(12) Uani d . . . 1.0 . .
H H44 0.2856 0.6561 0.6023 0.031 Uiso calc U . R 1.0 . .
C C45 0.2123(4) 0.4845(5) 0.61074(13) 0.0317(14) Uani d . . . 1.0 . .
H H45 0.2224 0.4926 0.6296 0.038 Uiso calc U . R 1.0 . .
C C46 0.1607(4) 0.3769(5) 0.59918(13) 0.0348(15) Uani d . . . 1.0 . .
H H46 0.1349 0.3109 0.6102 0.042 Uiso calc U . R 1.0 . .
C C47 0.1460(4) 0.3643(4) 0.57175(13) 0.0336(15) Uani d . . . 1.0 . .
H H47 0.1101 0.2899 0.5639 0.04 Uiso calc U . R 1.0 . .
C C48 0.1840(4) 0.4614(4) 0.55547(12) 0.0264(13) Uani d . . . 1.0 . .
H H48 0.1752 0.4528 0.5366 0.032 Uiso calc U . R 1.0 . .
O O3 0.8164(7) -0.0839(7) 0.55537(19) 0.060(2) Uani d U P D 0.620(9) A 1
C C49 0.8357(11) -0.0660(10) 0.6034(3) 0.072(4) Uani d U P D 0.620(9) A 1
H H49A 0.9188 -0.0131 0.6027 0.107 Uiso calc U P R 0.620(9) A 1
H H49B 0.8161 -0.1093 0.6203 0.107 Uiso calc U P R 0.620(9) A 1
H H49C 0.7956 -0.0221 0.6025 0.107 Uiso calc U P R 0.620(9) A 1
C C50 0.8001(12) -0.1475(11) 0.5802(3) 0.064(3) Uani d U P D 0.620(9) A 1
H H50A 0.8468 -0.1857 0.5799 0.077 Uiso calc U P R 0.620(9) A 1
H H50B 0.7184 -0.2075 0.5822 0.077 Uiso calc U P R 0.620(9) A 1
C C51 0.785(2) -0.1582(15) 0.5328(3) 0.061(4) Uani d U P D 0.620(9) A 1
H H51A 0.7076 -0.2258 0.5356 0.073 Uiso calc U P R 0.620(9) A 1
H H51B 0.8402 -0.1858 0.5305 0.073 Uiso calc U P R 0.620(9) A 1
C C52 0.7844(16) -0.0920(18) 0.5073(3) 0.098(6) Uani d U P D 0.620(9) A 1
H H52A 0.7251 -0.0704 0.509 0.147 Uiso calc U P R 0.620(9) A 1
H H52B 0.7683 -0.1412 0.4915 0.147 Uiso calc U P R 0.620(9) A 1
H H52C 0.8597 -0.0226 0.5052 0.147 Uiso calc U P R 0.620(9) A 1
O O3A 0.7927(11) -0.0567(11) 0.5323(3) 0.063(4) Uani d U P D 0.380(9) A 2
C C49A 0.847(3) -0.127(3) 0.5692(5) 0.096(8) Uani d U P D 0.380(9) A 2
H H49D 0.9214 -0.0558 0.5682 0.143 Uiso calc U P R 0.380(9) A 2
H H49E 0.8596 -0.1892 0.5758 0.143 Uiso calc U P R 0.380(9) A 2
H H49F 0.7965 -0.1172 0.5816 0.143 Uiso calc U P R 0.380(9) A 2
C C50A 0.793(4) -0.158(2) 0.5416(5) 0.054(5) Uani d U P D 0.380(9) A 2
H H50C 0.838 -0.1783 0.5294 0.065 Uiso calc U P R 0.380(9) A 2
H H50D 0.7135 -0.224 0.5426 0.065 Uiso calc U P R 0.380(9) A 2
C C51A 0.7512(15) -0.0653(15) 0.5051(3) 0.047(4) Uani d U P D 0.380(9) A 2
H H51C 0.809 -0.0629 0.4924 0.056 Uiso calc U P R 0.380(9) A 2
H H51D 0.6796 -0.1399 0.5028 0.056 Uiso calc U P R 0.380(9) A 2
C C52A 0.7293(13) 0.0255(15) 0.4991(5) 0.064(5) Uani d U P D 0.380(9) A 2
H H52D 0.6841 0.0328 0.5135 0.097 Uiso calc U P R 0.380(9) A 2
H H52E 0.6864 0.0086 0.4822 0.097 Uiso calc U P R 0.380(9) A 2
H H52F 0.8023 0.0977 0.4973 0.097 Uiso calc U P R 0.380(9) A 2
O O4 1.0849(7) 0.1846(6) 0.4453(2) 0.061(3) Uani d U P D 0.621(10) B 1
C C53 1.0675(10) 0.1643(11) 0.3970(3) 0.074(4) Uani d U P D 0.621(10) B 1
H H53A 1.0175 0.0806 0.3968 0.111 Uiso calc U P R 0.621(10) B 1
H H53B 1.1128 0.1889 0.3804 0.111 Uiso calc U P R 0.621(10) B 1
H H53C 1.0204 0.201 0.3983 0.111 Uiso calc U P R 0.621(10) B 1
C C54 1.1465(10) 0.1984(12) 0.4207(3) 0.064(4) Uani d U P D 0.621(10) B 1
H H54A 1.1833 0.1504 0.4213 0.077 Uiso calc U P R 0.621(10) B 1
H H54B 1.2078 0.2796 0.4187 0.077 Uiso calc U P R 0.621(10) B 1
C C55 1.1584(14) 0.2162(19) 0.4679(3) 0.058(4) Uani d U P D 0.621(10) B 1
H H55A 1.2246 0.2945 0.4653 0.07 Uiso calc U P R 0.621(10) B 1
H H55B 1.1882 0.1625 0.4699 0.07 Uiso calc U P R 0.621(10) B 1
C C56 1.0917(19) 0.2132(17) 0.4937(3) 0.105(6) Uani d U P D 0.621(10) B 1
H H56A 1.145 0.2699 0.5066 0.157 Uiso calc U P R 0.621(10) B 1
H H56B 1.0563 0.1364 0.5017 0.157 Uiso calc U P R 0.621(10) B 1
H H56C 1.0318 0.2315 0.4891 0.157 Uiso calc U P R 0.621(10) B 1
O O4A 0.0566(11) 0.2067(11) 0.4682(3) 0.065(4) Uani d U P D 0.379(10) B 2
C C53A 0.120(3) 0.145(3) 0.4316(6) 0.130(13) Uani d U P D 0.379(10) B 2
H H53D 0.0591 0.0653 0.4344 0.194 Uiso calc U P R 0.379(10) B 2
H H53E 0.1858 0.1462 0.4229 0.194 Uiso calc U P R 0.379(10) B 2
H H53F 0.091 0.1844 0.4202 0.194 Uiso calc U P R 0.379(10) B 2
C C54A 0.157(2) 0.206(4) 0.4586(5) 0.058(6) Uani d U P D 0.379(10) B 2
H H54C 0.1801 0.1639 0.4711 0.069 Uiso calc U P R 0.379(10) B 2
H H54D 0.2222 0.2853 0.4564 0.069 Uiso calc U P R 0.379(10) B 2
C C55A 0.0664(14) 0.2492(15) 0.4953(3) 0.047(5) Uani d U P D 0.379(10) B 2
H H55C 0.0609 0.191 0.5083 0.056 Uiso calc U P R 0.379(10) B 2
H H55D 0.1415 0.32 0.4977 0.056 Uiso calc U P R 0.379(10) B 2
C C56A -0.0235(15) 0.2727(14) 0.4997(5) 0.061(5) Uani d U P D 0.379(10) B 2
H H56D -0.0066 0.3435 0.4902 0.092 Uiso calc U P R 0.379(10) B 2
H H56E -0.0308 0.2822 0.5189 0.092 Uiso calc U P R 0.379(10) B 2
H H56F -0.0957 0.2088 0.4929 0.092 Uiso calc U P R 0.379(10) B 2
I I1 0.41793(3) 0.58206(3) 0.50027(2) 0.02466(8) Uani d . . . 1.0 . .
O O1 0.3721(3) 1.1098(3) 0.44452(7) 0.0311(9) Uani d . . . 1.0 . .
O O2 -0.1099(3) 0.6279(3) 0.55616(7) 0.0310(9) Uani d . . . 1.0 . .
P P1 0.30809(10) 0.73190(9) 0.45522(3) 0.0161(3) Uani d . . . 1.0 . .
P P2 0.26811(9) 0.69202(10) 0.54529(3) 0.0160(3) Uani d . . . 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 C1 . 2.038(4) ?
Pd1 P2 . 2.2872(14) ?
Pd1 P1 . 2.2890(14) ?
Pd1 I1 . 2.6708(4) ?
C1 C2 . 1.409(7) ?
C1 C6 . 1.410(7) ?
C2 C3 . 1.394(6) ?
C2 C28 . 1.510(7) ?
C3 C4 . 1.387(8) ?
C3 H3 . 0.95 ?
C4 C5 . 1.374(8) ?
C4 H4 . 0.95 ?
C5 C6 . 1.401(6) ?
C5 H5 . 0.95 ?
C6 C7 . 1.496(7) ?
C7 C8 . 1.547(6) ?
C7 P1 . 1.849(4) ?
C7 H7 . 1.0 ?
C8 C9 . 1.521(6) ?
C8 H8A . 0.99 ?
C8 H8B . 0.99 ?
C9 O1 . 1.215(6) ?
C9 C10 . 1.488(7) ?
C10 C15 . 1.385(7) ?
C10 C11 . 1.395(6) ?
C11 C12 . 1.372(8) ?
C11 H11 . 0.95 ?
C12 C13 . 1.383(8) ?
C12 H12 . 0.95 ?
C13 C14 . 1.380(7) ?
C13 H13 . 0.95 ?
C14 C15 . 1.373(7) ?
C14 H14 . 0.95 ?
C15 H15 . 0.95 ?
C16 C17 . 1.385(7) ?
C16 C21 . 1.393(7) ?
C16 P1 . 1.822(5) ?
C17 C18 . 1.401(7) ?
C17 H17 . 0.95 ?
C18 C19 . 1.385(8) ?
C18 H18 . 0.95 ?
C19 C20 . 1.378(8) ?
C19 H19 . 0.95 ?
C20 C21 . 1.391(7) ?
C20 H20 . 0.95 ?
C21 H21 . 0.95 ?
C22 C27 . 1.395(6) ?
C22 C23 . 1.401(7) ?
C22 P1 . 1.819(5) ?
C23 C24 . 1.385(6) ?
C23 H23 . 0.95 ?
C24 C25 . 1.379(6) ?
C24 H24 . 0.95 ?
C25 C26 . 1.387(7) ?
C25 H25 . 0.95 ?
C26 C27 . 1.388(7) ?
C26 H26 . 0.95 ?
C27 H27 . 0.95 ?
C28 C29 . 1.552(6) ?
C28 P2 . 1.843(4) ?
C28 H28 . 1.0 ?
C29 C30 . 1.530(6) ?
C29 H29A . 0.99 ?
C29 H29B . 0.99 ?
C30 O2 . 1.219(6) ?
C30 C31 . 1.482(7) ?
C31 C32 . 1.389(6) ?
C31 C36 . 1.391(7) ?
C32 C33 . 1.370(8) ?
C32 H32 . 0.95 ?
C33 C34 . 1.378(8) ?
C33 H33 . 0.95 ?
C34 C35 . 1.382(7) ?
C34 H34 . 0.95 ?
C35 C36 . 1.375(8) ?
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?
C37 C38 . 1.395(6) ?
C37 C42 . 1.402(7) ?
C37 P2 . 1.817(5) ?
C38 C39 . 1.391(7) ?
C38 H38 . 0.95 ?
C39 C40 . 1.385(7) ?
C39 H39 . 0.95 ?
C40 C41 . 1.383(6) ?
C40 H40 . 0.95 ?
C41 C42 . 1.385(6) ?
C41 H41 . 0.95 ?
C42 H42 . 0.95 ?
C43 C48 . 1.387(7) ?
C43 C44 . 1.389(7) ?
C43 P2 . 1.819(5) ?
C44 C45 . 1.403(7) ?
C44 H44 . 0.95 ?
C45 C46 . 1.378(8) ?
C45 H45 . 0.95 ?
C46 C47 . 1.380(8) ?
C46 H46 . 0.95 ?
C47 C48 . 1.398(7) ?
C47 H47 . 0.95 ?
C48 H48 . 0.95 ?
O3 C51 . 1.422(14) ?
O3 C50 . 1.459(13) ?
C49 C50 . 1.496(13) ?
C49 H49A . 0.98 ?
C49 H49B . 0.98 ?
C49 H49C . 0.98 ?
C50 H50A . 0.99 ?
C50 H50B . 0.99 ?
C51 C52 . 1.555(15) ?
C51 H51A . 0.99 ?
C51 H51B . 0.99 ?
C52 H52A . 0.98 ?
C52 H52B . 0.98 ?
C52 H52C . 0.98 ?
O3A C50A . 1.440(18) ?
O3A C51A . 1.445(17) ?
C49A C50A . 1.52(2) ?
C49A H49D . 0.98 ?
C49A H49E . 0.98 ?
C49A H49F . 0.98 ?
C50A H50C . 0.99 ?
C50A H50D . 0.99 ?
C51A C52A . 1.424(17) ?
C51A H51C . 0.99 ?
C51A H51D . 0.99 ?
C52A H52D . 0.98 ?
C52A H52E . 0.98 ?
C52A H52F . 0.98 ?
O4 C55 . 1.417(14) ?
O4 C54 . 1.442(13) ?
C53 C54 . 1.498(13) ?
C53 H53A . 0.98 ?
C53 H53B . 0.98 ?
C53 H53C . 0.98 ?
C54 H54A . 0.99 ?
C54 H54B . 0.99 ?
C55 C56 . 1.557(15) ?
C55 H55A . 0.99 ?
C55 H55B . 0.99 ?
C56 H56A . 0.98 ?
C56 H56B . 0.98 ?
C56 H56C . 0.98 ?
O4A C54A . 1.438(18) ?
O4A C55A . 1.446(17) ?
C53A C54A . 1.52(2) ?
C53A H53D . 0.98 ?
C53A H53E . 0.98 ?
C53A H53F . 0.98 ?
C54A H54C . 0.99 ?
C54A H54D . 0.99 ?
C55A C56A . 1.411(17) ?
C55A H55C . 0.99 ?
C55A H55D . 0.99 ?
C56A H56D . 0.98 ?
C56A H56E . 0.98 ?
C56A H56F . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Pd1 P2 . . 81.19(17) ?
C1 Pd1 P1 . . 81.05(17) ?
P2 Pd1 P1 . . 162.24(4) ?
C1 Pd1 I1 . . 179.88(18) ?
P2 Pd1 I1 . . 98.90(3) ?
P1 Pd1 I1 . . 98.86(3) ?
C2 C1 C6 . . 118.3(3) ?
C2 C1 Pd1 . . 120.8(4) ?
C6 C1 Pd1 . . 120.9(4) ?
C3 C2 C1 . . 120.2(4) ?
C3 C2 C28 . . 120.5(4) ?
C1 C2 C28 . . 119.2(4) ?
C4 C3 C2 . . 120.9(5) ?
C4 C3 H3 . . 119.5 ?
C2 C3 H3 . . 119.5 ?
C5 C4 C3 . . 119.5(4) ?
C5 C4 H4 . . 120.3 ?
C3 C4 H4 . . 120.3 ?
C4 C5 C6 . . 121.0(5) ?
C4 C5 H5 . . 119.5 ?
C6 C5 H5 . . 119.5 ?
C5 C6 C1 . . 120.0(4) ?
C5 C6 C7 . . 120.6(4) ?
C1 C6 C7 . . 119.2(4) ?
C6 C7 C8 . . 111.2(4) ?
C6 C7 P1 . . 104.9(3) ?
C8 C7 P1 . . 109.0(3) ?
C6 C7 H7 . . 110.5 ?
C8 C7 H7 . . 110.5 ?
P1 C7 H7 . . 110.5 ?
C9 C8 C7 . . 109.4(4) ?
C9 C8 H8A . . 109.8 ?
C7 C8 H8A . . 109.8 ?
C9 C8 H8B . . 109.8 ?
C7 C8 H8B . . 109.8 ?
H8A C8 H8B . . 108.2 ?
O1 C9 C10 . . 120.7(4) ?
O1 C9 C8 . . 119.0(5) ?
C10 C9 C8 . . 120.2(4) ?
C15 C10 C11 . . 118.7(5) ?
C15 C10 C9 . . 122.7(4) ?
C11 C10 C9 . . 118.6(4) ?
C12 C11 C10 . . 120.7(5) ?
C12 C11 H11 . . 119.6 ?
C10 C11 H11 . . 119.6 ?
C11 C12 C13 . . 120.4(5) ?
C11 C12 H12 . . 119.8 ?
C13 C12 H12 . . 119.8 ?
C14 C13 C12 . . 118.7(5) ?
C14 C13 H13 . . 120.6 ?
C12 C13 H13 . . 120.6 ?
C15 C14 C13 . . 121.4(5) ?
C15 C14 H14 . . 119.3 ?
C13 C14 H14 . . 119.3 ?
C14 C15 C10 . . 120.0(4) ?
C14 C15 H15 . . 120.0 ?
C10 C15 H15 . . 120.0 ?
C17 C16 C21 . . 119.7(5) ?
C17 C16 P1 . . 121.8(4) ?
C21 C16 P1 . . 118.3(4) ?
C16 C17 C18 . . 120.1(5) ?
C16 C17 H17 . . 119.9 ?
C18 C17 H17 . . 119.9 ?
C19 C18 C17 . . 119.5(6) ?
C19 C18 H18 . . 120.3 ?
C17 C18 H18 . . 120.3 ?
C20 C19 C18 . . 120.7(5) ?
C20 C19 H19 . . 119.7 ?
C18 C19 H19 . . 119.7 ?
C19 C20 C21 . . 119.9(5) ?
C19 C20 H20 . . 120.1 ?
C21 C20 H20 . . 120.1 ?
C20 C21 C16 . . 120.1(6) ?
C20 C21 H21 . . 119.9 ?
C16 C21 H21 . . 119.9 ?
C27 C22 C23 . . 119.1(4) ?
C27 C22 P1 . . 117.9(4) ?
C23 C22 P1 . . 122.9(3) ?
C24 C23 C22 . . 120.0(4) ?
C24 C23 H23 . . 120.0 ?
C22 C23 H23 . . 120.0 ?
C25 C24 C23 . . 120.4(5) ?
C25 C24 H24 . . 119.8 ?
C23 C24 H24 . . 119.8 ?
C24 C25 C26 . . 120.2(4) ?
C24 C25 H25 . . 119.9 ?
C26 C25 H25 . . 119.9 ?
C25 C26 C27 . . 119.9(4) ?
C25 C26 H26 . . 120.0 ?
C27 C26 H26 . . 120.0 ?
C26 C27 C22 . . 120.3(5) ?
C26 C27 H27 . . 119.8 ?
C22 C27 H27 . . 119.8 ?
C2 C28 C29 . . 110.6(4) ?
C2 C28 P2 . . 104.7(3) ?
C29 C28 P2 . . 108.9(3) ?
C2 C28 H28 . . 110.8 ?
C29 C28 H28 . . 110.8 ?
P2 C28 H28 . . 110.8 ?
C30 C29 C28 . . 109.4(4) ?
C30 C29 H29A . . 109.8 ?
C28 C29 H29A . . 109.8 ?
C30 C29 H29B . . 109.8 ?
C28 C29 H29B . . 109.8 ?
H29A C29 H29B . . 108.2 ?
O2 C30 C31 . . 121.1(4) ?
O2 C30 C29 . . 118.8(5) ?
C31 C30 C29 . . 120.0(4) ?
C32 C31 C36 . . 118.6(5) ?
C32 C31 C30 . . 118.7(4) ?
C36 C31 C30 . . 122.7(4) ?
C33 C32 C31 . . 121.5(5) ?
C33 C32 H32 . . 119.3 ?
C31 C32 H32 . . 119.3 ?
C32 C33 C34 . . 119.8(5) ?
C32 C33 H33 . . 120.1 ?
C34 C33 H33 . . 120.1 ?
C33 C34 C35 . . 119.4(5) ?
C33 C34 H34 . . 120.3 ?
C35 C34 H34 . . 120.3 ?
C36 C35 C34 . . 121.2(5) ?
C36 C35 H35 . . 119.4 ?
C34 C35 H35 . . 119.4 ?
C35 C36 C31 . . 119.7(4) ?
C35 C36 H36 . . 120.2 ?
C31 C36 H36 . . 120.2 ?
C38 C37 C42 . . 119.1(4) ?
C38 C37 P2 . . 117.8(4) ?
C42 C37 P2 . . 123.2(3) ?
C39 C38 C37 . . 120.2(5) ?
C39 C38 H38 . . 119.9 ?
C37 C38 H38 . . 119.9 ?
C40 C39 C38 . . 120.2(4) ?
C40 C39 H39 . . 119.9 ?
C38 C39 H39 . . 119.9 ?
C41 C40 C39 . . 119.8(4) ?
C41 C40 H40 . . 120.1 ?
C39 C40 H40 . . 120.1 ?
C40 C41 C42 . . 120.6(5) ?
C40 C41 H41 . . 119.7 ?
C42 C41 H41 . . 119.7 ?
C41 C42 C37 . . 120.0(4) ?
C41 C42 H42 . . 120.0 ?
C37 C42 H42 . . 120.0 ?
C48 C43 C44 . . 119.5(5) ?
C48 C43 P2 . . 118.6(4) ?
C44 C43 P2 . . 121.7(4) ?
C43 C44 C45 . . 120.2(5) ?
C43 C44 H44 . . 119.9 ?
C45 C44 H44 . . 119.9 ?
C46 C45 C44 . . 119.6(6) ?
C46 C45 H45 . . 120.2 ?
C44 C45 H45 . . 120.2 ?
C45 C46 C47 . . 120.6(5) ?
C45 C46 H46 . . 119.7 ?
C47 C46 H46 . . 119.7 ?
C46 C47 C48 . . 119.8(5) ?
C46 C47 H47 . . 120.1 ?
C48 C47 H47 . . 120.1 ?
C43 C48 C47 . . 120.2(6) ?
C43 C48 H48 . . 119.9 ?
C47 C48 H48 . . 119.9 ?
C51 O3 C50 . . 110.8(10) ?
C50 C49 H49A . . 109.5 ?
C50 C49 H49B . . 109.5 ?
H49A C49 H49B . . 109.5 ?
C50 C49 H49C . . 109.5 ?
H49A C49 H49C . . 109.5 ?
H49B C49 H49C . . 109.5 ?
O3 C50 C49 . . 109.0(10) ?
O3 C50 H50A . . 109.9 ?
C49 C50 H50A . . 109.9 ?
O3 C50 H50B . . 109.9 ?
C49 C50 H50B . . 109.9 ?
H50A C50 H50B . . 108.3 ?
O3 C51 C52 . . 109.3(13) ?
O3 C51 H51A . . 109.8 ?
C52 C51 H51A . . 109.8 ?
O3 C51 H51B . . 109.8 ?
C52 C51 H51B . . 109.8 ?
H51A C51 H51B . . 108.3 ?
C51 C52 H52A . . 109.5 ?
C51 C52 H52B . . 109.5 ?
H52A C52 H52B . . 109.5 ?
C51 C52 H52C . . 109.5 ?
H52A C52 H52C . . 109.5 ?
H52B C52 H52C . . 109.5 ?
C50A O3A C51A . . 114.2(15) ?
C50A C49A H49D . . 109.5 ?
C50A C49A H49E . . 109.5 ?
H49D C49A H49E . . 109.5 ?
C50A C49A H49F . . 109.5 ?
H49D C49A H49F . . 109.5 ?
H49E C49A H49F . . 109.5 ?
O3A C50A C49A . . 105.3(18) ?
O3A C50A H50C . . 110.7 ?
C49A C50A H50C . . 110.7 ?
O3A C50A H50D . . 110.7 ?
C49A C50A H50D . . 110.7 ?
H50C C50A H50D . . 108.8 ?
C52A C51A O3A . . 111.6(15) ?
C52A C51A H51C . . 109.3 ?
O3A C51A H51C . . 109.3 ?
C52A C51A H51D . . 109.3 ?
O3A C51A H51D . . 109.3 ?
H51C C51A H51D . . 108.0 ?
C51A C52A H52D . . 109.5 ?
C51A C52A H52E . . 109.5 ?
H52D C52A H52E . . 109.5 ?
C51A C52A H52F . . 109.5 ?
H52D C52A H52F . . 109.5 ?
H52E C52A H52F . . 109.5 ?
C55 O4 C54 . . 111.7(10) ?
C54 C53 H53A . . 109.5 ?
C54 C53 H53B . . 109.5 ?
H53A C53 H53B . . 109.5 ?
C54 C53 H53C . . 109.5 ?
H53A C53 H53C . . 109.5 ?
H53B C53 H53C . . 109.5 ?
O4 C54 C53 . . 111.0(10) ?
O4 C54 H54A . . 109.4 ?
C53 C54 H54A . . 109.4 ?
O4 C54 H54B . . 109.4 ?
C53 C54 H54B . . 109.4 ?
H54A C54 H54B . . 108.0 ?
O4 C55 C56 . . 110.1(13) ?
O4 C55 H55A . . 109.6 ?
C56 C55 H55A . . 109.6 ?
O4 C55 H55B . . 109.6 ?
C56 C55 H55B . . 109.6 ?
H55A C55 H55B . . 108.2 ?
C55 C56 H56A . . 109.5 ?
C55 C56 H56B . . 109.5 ?
H56A C56 H56B . . 109.5 ?
C55 C56 H56C . . 109.5 ?
H56A C56 H56C . . 109.5 ?
H56B C56 H56C . . 109.5 ?
C54A O4A C55A . . 114.4(15) ?
C54A C53A H53D . . 109.5 ?
C54A C53A H53E . . 109.5 ?
H53D C53A H53E . . 109.5 ?
C54A C53A H53F . . 109.5 ?
H53D C53A H53F . . 109.5 ?
H53E C53A H53F . . 109.5 ?
O4A C54A C53A . . 103.9(19) ?
O4A C54A H54C . . 111.0 ?
C53A C54A H54C . . 111.0 ?
O4A C54A H54D . . 111.0 ?
C53A C54A H54D . . 111.0 ?
H54C C54A H54D . . 109.0 ?
C56A C55A O4A . . 108.4(14) ?
C56A C55A H55C . . 110.0 ?
O4A C55A H55C . . 110.0 ?
C56A C55A H55D . . 110.0 ?
O4A C55A H55D . . 110.0 ?
H55C C55A H55D . . 108.4 ?
C55A C56A H56D . . 109.5 ?
C55A C56A H56E . . 109.5 ?
H56D C56A H56E . . 109.5 ?
C55A C56A H56F . . 109.5 ?
H56D C56A H56F . . 109.5 ?
H56E C56A H56F . . 109.5 ?
C22 P1 C16 . . 105.7(2) ?
C22 P1 C7 . . 107.3(2) ?
C16 P1 C7 . . 104.8(2) ?
C22 P1 Pd1 . . 111.97(16) ?
C16 P1 Pd1 . . 124.10(17) ?
C7 P1 Pd1 . . 101.70(17) ?
C37 P2 C43 . . 105.8(2) ?
C37 P2 C28 . . 107.1(2) ?
C43 P2 C28 . . 104.5(2) ?
C37 P2 Pd1 . . 112.08(17) ?
C43 P2 Pd1 . . 123.98(18) ?
C28 P2 Pd1 . . 102.06(17) ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/DEE'
_database_code_depnum_ccdc_archive 'CCDC 1019491'
#######################################################################
#
#                 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
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_leung700s

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_absolute_configuration ad
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H41 Cl3 O8 P2 Pd'
_chemical_formula_weight         960.45

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P2(1)2(1)2(1) '

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

_cell_length_a                   10.4536(4)
_cell_length_b                   17.2754(6)
_cell_length_c                   24.4730(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4419.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9946
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      31.75
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1960
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7607
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63361
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         37.57
_reflns_number_total             23124
_reflns_number_gt                18774
_reflns_threshold_expression     >2sigma(I)

_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_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)+(0.0373P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(12)
_refine_ls_number_reflns         23124
_refine_ls_number_parameters     547
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0776
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.003
_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
Pd1 Pd 0.569064(12) 0.412996(8) 0.841305(5) 0.01324(3) Uani 1 1 d . . .
C1 C 0.75959(16) 0.42461(11) 0.85148(6) 0.0146(3) Uani 1 1 d . . .
C2 C 0.84412(17) 0.40108(11) 0.80969(7) 0.0167(3) Uani 1 1 d . . .
C3 C 0.97606(17) 0.40433(13) 0.81759(8) 0.0224(4) Uani 1 1 d . . .
H3 H 1.0321 0.3894 0.7889 0.027 Uiso 1 1 calc R . .
C4 C 1.02615(18) 0.42925(13) 0.86724(8) 0.0243(4) Uani 1 1 d . . .
H4 H 1.1161 0.4312 0.8726 0.029 Uiso 1 1 calc R . .
C5 C 0.94458(19) 0.45115(12) 0.90866(8) 0.0214(4) Uani 1 1 d . . .
H5 H 0.9788 0.4671 0.9428 0.026 Uiso 1 1 calc R . .
C6 C 0.81263(17) 0.45024(11) 0.90111(7) 0.0157(3) Uani 1 1 d . . .
C7 C 0.72449(17) 0.47711(11) 0.94625(7) 0.0152(3) Uani 1 1 d . . .
H7 H 0.7622 0.4633 0.9825 0.018 Uiso 1 1 calc R . .
C8 C 0.69602(19) 0.56495(11) 0.94451(7) 0.0181(3) Uani 1 1 d D A .
H8 H 0.6219 0.5749 0.9196 0.022 Uiso 1 1 calc R . .
C9 C 0.8133(2) 0.60850(12) 0.92360(8) 0.0231(4) Uani 1 1 d . . .
C10 C 0.9183(3) 0.65277(17) 0.84464(12) 0.0449(7) Uani 1 1 d . . .
H10A H 0.9408 0.7019 0.8622 0.067 Uiso 1 1 calc R . .
H10B H 0.9014 0.6617 0.8058 0.067 Uiso 1 1 calc R . .
H10C H 0.9894 0.6162 0.8486 0.067 Uiso 1 1 calc R . .
C11 C 0.6655(2) 0.59566(13) 1.00124(8) 0.0255(4) Uani 1 1 d D . .
C13 C 0.44840(18) 0.46369(11) 0.97311(7) 0.0179(3) Uani 1 1 d . . .
C14 C 0.4400(3) 0.45787(15) 1.02966(8) 0.0331(5) Uani 1 1 d . . .
H14 H 0.5029 0.4299 1.0495 0.040 Uiso 1 1 calc R . .
C15 C 0.3395(3) 0.4930(2) 1.05699(11) 0.0505(8) Uani 1 1 d . . .
H15 H 0.3332 0.4881 1.0956 0.061 Uiso 1 1 calc R . .
C16 C 0.2489(3) 0.53502(18) 1.02909(12) 0.0466(7) Uani 1 1 d . . .
H16 H 0.1816 0.5597 1.0485 0.056 Uiso 1 1 calc R . .
C17 C 0.2554(2) 0.54143(15) 0.97307(11) 0.0355(5) Uani 1 1 d . . .
H17 H 0.1927 0.5703 0.9537 0.043 Uiso 1 1 calc R . .
C18 C 0.3551(2) 0.50508(13) 0.94504(9) 0.0248(4) Uani 1 1 d . . .
H18 H 0.3592 0.5087 0.9063 0.030 Uiso 1 1 calc R . .
C19 C 0.60963(19) 0.32609(12) 0.96603(8) 0.0197(4) Uani 1 1 d . . .
C20 C 0.6828(2) 0.31687(14) 1.01359(9) 0.0284(5) Uani 1 1 d . . .
H20 H 0.7169 0.3610 1.0316 0.034 Uiso 1 1 calc R . .
C21 C 0.7057(3) 0.24333(15) 1.03445(11) 0.0357(6) Uani 1 1 d . . .
H21 H 0.7555 0.2373 1.0666 0.043 Uiso 1 1 calc R . .
C22 C 0.6561(3) 0.17880(15) 1.00849(12) 0.0394(6) Uani 1 1 d . . .
H22 H 0.6718 0.1286 1.0229 0.047 Uiso 1 1 calc R . .
C23 C 0.5838(3) 0.18736(14) 0.96172(12) 0.0406(6) Uani 1 1 d . . .
H23 H 0.5497 0.1429 0.9441 0.049 Uiso 1 1 calc R . .
C24 C 0.5606(2) 0.26058(12) 0.94015(9) 0.0296(4) Uani 1 1 d . . .
H24 H 0.5113 0.2659 0.9078 0.036 Uiso 1 1 calc R . .
C25 C 0.78743(18) 0.36649(11) 0.75814(7) 0.0177(3) Uani 1 1 d . . .
H25 H 0.8432 0.3767 0.7257 0.021 Uiso 1 1 calc R . .
C26 C 0.75906(19) 0.27815(12) 0.76442(7) 0.0189(3) Uani 1 1 d . . .
H26 H 0.6730 0.2717 0.7816 0.023 Uiso 1 1 calc R . .
C27 C 0.8587(2) 0.24071(13) 0.80103(8) 0.0244(4) Uani 1 1 d . . .
C28 C 0.9108(3) 0.21637(19) 0.89278(11) 0.0492(8) Uani 1 1 d . . .
H28A H 0.9415 0.1640 0.8847 0.074 Uiso 1 1 calc R . .
H28B H 0.8713 0.2172 0.9291 0.074 Uiso 1 1 calc R . .
H28C H 0.9830 0.2526 0.8920 0.074 Uiso 1 1 calc R . .
C29 C 0.7601(2) 0.23559(13) 0.71031(8) 0.0255(4) Uani 1 1 d . . .
C30 C 0.6843(3) 0.12276(18) 0.66691(12) 0.0523(8) Uani 1 1 d . . .
H30A H 0.6527 0.1536 0.6362 0.079 Uiso 1 1 calc R . .
H30B H 0.6257 0.0795 0.6736 0.079 Uiso 1 1 calc R . .
H30C H 0.7695 0.1026 0.6582 0.079 Uiso 1 1 calc R . .
C31 C 0.55003(18) 0.36567(12) 0.69581(7) 0.0186(4) Uani 1 1 d . . .
C32 C 0.4634(2) 0.30665(14) 0.70771(9) 0.0258(4) Uani 1 1 d . . .
H32 H 0.4436 0.2950 0.7447 0.031 Uiso 1 1 calc R . .
C33 C 0.4058(2) 0.26479(15) 0.66606(11) 0.0367(6) Uani 1 1 d . . .
H33 H 0.3463 0.2249 0.6744 0.044 Uiso 1 1 calc R . .
C34 C 0.4360(3) 0.28175(16) 0.61170(10) 0.0419(6) Uani 1 1 d . . .
H34 H 0.3978 0.2529 0.5830 0.050 Uiso 1 1 calc R . .
C35 C 0.5212(3) 0.34015(17) 0.59977(9) 0.0371(6) Uani 1 1 d . . .
H35 H 0.5403 0.3518 0.5627 0.045 Uiso 1 1 calc R . .
C36 C 0.5796(2) 0.38238(13) 0.64130(8) 0.0260(4) Uani 1 1 d . . .
H36 H 0.6390 0.4222 0.6327 0.031 Uiso 1 1 calc R . .
C37 C 0.6576(2) 0.51147(12) 0.72460(8) 0.0209(4) Uani 1 1 d . . .
C38 C 0.5503(3) 0.55818(14) 0.71766(12) 0.0393(6) Uani 1 1 d . . .
H38 H 0.4683 0.5388 0.7273 0.047 Uiso 1 1 calc R . .
C39 C 0.5614(4) 0.63285(15) 0.69682(13) 0.0520(8) Uani 1 1 d . . .
H39 H 0.4874 0.6639 0.6914 0.062 Uiso 1 1 calc R . .
C40 C 0.6812(4) 0.66123(16) 0.68407(12) 0.0494(8) Uani 1 1 d . . .
H40 H 0.6903 0.7124 0.6704 0.059 Uiso 1 1 calc R . .
C41 C 0.7865(3) 0.61563(18) 0.69111(13) 0.0506(8) Uani 1 1 d . . .
H41 H 0.8686 0.6354 0.6820 0.061 Uiso 1 1 calc R . .
C42 C 0.7758(3) 0.54119(17) 0.71121(12) 0.0407(7) Uani 1 1 d . . .
H42 H 0.8503 0.5103 0.7158 0.049 Uiso 1 1 calc R . .
C43 C 0.2172(3) 0.43736(17) 0.69993(11) 0.0403(6) Uani 1 1 d . . .
H43A H 0.2530 0.4162 0.7343 0.048 Uiso 1 1 calc R . .
H43B H 0.2874 0.4403 0.6729 0.048 Uiso 1 1 calc R . .
Cl1 Cl 0.34703(4) 0.38541(3) 0.83144(2) 0.02674(11) Uani 1 1 d . . .
Cl2 Cl 0.15779(9) 0.53045(5) 0.71204(3) 0.05118(19) Uani 1 1 d . . .
Cl3 Cl 0.09798(8) 0.37465(5) 0.67547(3) 0.05166(19) Uani 1 1 d . . .
O1 O 0.80444(16) 0.62089(10) 0.87042(6) 0.0280(3) Uani 1 1 d . . .
O2 O 0.90288(17) 0.62620(11) 0.95228(7) 0.0383(4) Uani 1 1 d . . .
C12 C 0.548(3) 0.6964(11) 1.0469(8) 0.053(4) Uani 0.44(5) 1 d PDU A 1
H12A H 0.4838 0.6644 1.0651 0.080 Uiso 0.44(5) 1 calc PR A 1
H12B H 0.5113 0.7468 1.0376 0.080 Uiso 0.44(5) 1 calc PR A 1
H12C H 0.6215 0.7038 1.0714 0.080 Uiso 0.44(5) 1 calc PR A 1
O3 O 0.591(2) 0.6578(9) 0.9972(6) 0.037(3) Uani 0.44(5) 1 d PDU A 1
O4 O 0.709(2) 0.5673(12) 1.0420(6) 0.030(3) Uani 0.44(5) 1 d PDU A 1
C12A C 0.599(2) 0.7048(10) 1.0508(5) 0.049(3) Uani 0.56(5) 1 d PDU A 2
H12D H 0.5476 0.6708 1.0743 0.073 Uiso 0.56(5) 1 calc PR A 2
H12E H 0.5536 0.7539 1.0454 0.073 Uiso 0.56(5) 1 calc PR A 2
H12F H 0.6817 0.7147 1.0681 0.073 Uiso 0.56(5) 1 calc PR A 2
O3A O 0.6190(18) 0.6674(6) 0.9981(4) 0.034(2) Uani 0.56(5) 1 d PDU A 2
O4A O 0.6813(17) 0.5615(9) 1.0441(5) 0.032(2) Uani 0.56(5) 1 d PDU A 2
O5 O 0.81751(16) 0.23903(10) 0.85234(6) 0.0305(4) Uani 1 1 d . . .
O6 O 0.96037(17) 0.21774(12) 0.78565(7) 0.0393(4) Uani 1 1 d . . .
O7 O 0.6916(2) 0.17083(10) 0.71527(7) 0.0384(4) Uani 1 1 d . . .
O8 O 0.81430(19) 0.25588(11) 0.66989(6) 0.0376(4) Uani 1 1 d . . .
P1 P 0.57746(4) 0.41935(3) 0.934592(16) 0.01434(8) Uani 1 1 d . . .
P2 P 0.63122(4) 0.41508(3) 0.751099(17) 0.01496(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.0172(17) . ?
Pd1 P1 2.2873(4) . ?
Pd1 P2 2.3015(4) . ?
Pd1 Cl1 2.3818(5) . ?
C1 C6 1.407(2) . ?
C1 C2 1.411(2) . ?
C2 C3 1.394(3) . ?
C2 C25 1.517(3) . ?
C3 C4 1.391(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.511(2) . ?
C7 C8 1.547(3) . ?
C7 P1 1.8546(18) . ?
C7 H7 1.0000 . ?
C8 C11 1.520(3) . ?
C8 C9 1.527(3) . ?
C8 H8 1.0000 . ?
C9 O2 1.209(3) . ?
C9 O1 1.322(3) . ?
C10 O1 1.455(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 O4 1.202(10) . ?
C11 O4A 1.215(8) . ?
C11 O3 1.331(10) . ?
C11 O3A 1.334(7) . ?
C13 C14 1.391(3) . ?
C13 C18 1.391(3) . ?
C13 P1 1.8153(19) . ?
C14 C15 1.385(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.375(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.397(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.394(3) . ?
C19 C20 1.402(3) . ?
C19 P1 1.817(2) . ?
C20 C21 1.390(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.384(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.562(3) . ?
C25 P2 1.8442(19) . ?
C25 H25 1.0000 . ?
C26 C29 1.515(3) . ?
C26 C27 1.518(3) . ?
C26 H26 1.0000 . ?
C27 O6 1.196(3) . ?
C27 O5 1.328(3) . ?
C28 O5 1.444(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 O8 1.193(3) . ?
C29 O7 1.333(3) . ?
C30 O7 1.448(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.395(3) . ?
C31 C36 1.399(3) . ?
C31 P2 1.8110(18) . ?
C32 C33 1.387(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.398(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.376(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.392(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.378(3) . ?
C37 C38 1.392(3) . ?
C37 P2 1.808(2) . ?
C38 C39 1.392(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.381(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.365(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.381(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 Cl2 1.749(3) . ?
C43 Cl3 1.757(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C12 O3 1.457(11) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12A O3A 1.458(8) . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 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
C1 Pd1 P1 80.45(5) . . ?
C1 Pd1 P2 80.69(5) . . ?
P1 Pd1 P2 161.052(18) . . ?
C1 Pd1 Cl1 174.05(5) . . ?
P1 Pd1 Cl1 98.521(17) . . ?
P2 Pd1 Cl1 100.426(17) . . ?
C6 C1 C2 118.01(15) . . ?
C6 C1 Pd1 121.81(12) . . ?
C2 C1 Pd1 120.00(12) . . ?
C3 C2 C1 120.49(16) . . ?
C3 C2 C25 121.19(16) . . ?
C1 C2 C25 118.15(16) . . ?
C4 C3 C2 120.39(17) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C4 C3 119.64(18) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.85(18) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 120.59(16) . . ?
C5 C6 C7 120.24(16) . . ?
C1 C6 C7 119.17(15) . . ?
C6 C7 C8 113.48(15) . . ?
C6 C7 P1 103.16(12) . . ?
C8 C7 P1 111.35(13) . . ?
C6 C7 H7 109.6 . . ?
C8 C7 H7 109.6 . . ?
P1 C7 H7 109.6 . . ?
C11 C8 C9 107.61(16) . . ?
C11 C8 C7 110.95(16) . . ?
C9 C8 C7 109.76(16) . . ?
C11 C8 H8 109.5 . . ?
C9 C8 H8 109.5 . . ?
C7 C8 H8 109.5 . . ?
O2 C9 O1 125.8(2) . . ?
O2 C9 C8 123.50(19) . . ?
O1 C9 C8 110.69(17) . . ?
O1 C10 H10A 109.5 . . ?
O1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O4 C11 O4A 14.9(13) . . ?
O4 C11 O3 127.9(11) . . ?
O4A C11 O3 122.5(11) . . ?
O4 C11 O3A 124.5(12) . . ?
O4A C11 O3A 123.5(9) . . ?
O3 C11 O3A 14.6(13) . . ?
O4 C11 C8 122.4(10) . . ?
O4A C11 C8 126.2(9) . . ?
O3 C11 C8 109.6(6) . . ?
O3A C11 C8 110.3(5) . . ?
C14 C13 C18 118.96(19) . . ?
C14 C13 P1 122.25(16) . . ?
C18 C13 P1 118.80(14) . . ?
C15 C14 C13 119.8(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 120.9(2) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.2(2) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C16 C17 C18 119.3(2) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C13 C18 C17 120.8(2) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C24 C19 C20 119.0(2) . . ?
C24 C19 P1 117.34(16) . . ?
C20 C19 P1 123.60(17) . . ?
C21 C20 C19 120.2(2) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 120.2(2) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C21 120.0(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.5(2) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C19 120.1(2) . . ?
C23 C24 H24 120.0 . . ?
C19 C24 H24 120.0 . . ?
C2 C25 C26 112.16(15) . . ?
C2 C25 P2 104.14(12) . . ?
C26 C25 P2 106.60(13) . . ?
C2 C25 H25 111.2 . . ?
C26 C25 H25 111.2 . . ?
P2 C25 H25 111.2 . . ?
C29 C26 C27 107.71(16) . . ?
C29 C26 C25 112.76(16) . . ?
C27 C26 C25 110.12(17) . . ?
C29 C26 H26 108.7 . . ?
C27 C26 H26 108.7 . . ?
C25 C26 H26 108.7 . . ?
O6 C27 O5 125.4(2) . . ?
O6 C27 C26 124.4(2) . . ?
O5 C27 C26 110.19(18) . . ?
O5 C28 H28A 109.5 . . ?
O5 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O5 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O8 C29 O7 125.2(2) . . ?
O8 C29 C26 125.8(2) . . ?
O7 C29 C26 108.90(18) . . ?
O7 C30 H30A 109.5 . . ?
O7 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O7 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C36 119.55(18) . . ?
C32 C31 P2 119.54(15) . . ?
C36 C31 P2 120.77(16) . . ?
C33 C32 C31 120.6(2) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 119.4(2) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C35 C34 C33 120.1(2) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.9(2) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C35 C36 C31 119.4(2) . . ?
C35 C36 H36 120.3 . . ?
C31 C36 H36 120.3 . . ?
C42 C37 C38 118.5(2) . . ?
C42 C37 P2 124.40(19) . . ?
C38 C37 P2 117.07(17) . . ?
C37 C38 C39 121.0(3) . . ?
C37 C38 H38 119.5 . . ?
C39 C38 H38 119.5 . . ?
C40 C39 C38 119.2(3) . . ?
C40 C39 H39 120.4 . . ?
C38 C39 H39 120.4 . . ?
C41 C40 C39 119.9(3) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C40 C41 C42 121.1(3) . . ?
C40 C41 H41 119.4 . . ?
C42 C41 H41 119.4 . . ?
C37 C42 C41 120.3(3) . . ?
C37 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
Cl2 C43 Cl3 111.87(16) . . ?
Cl2 C43 H43A 109.2 . . ?
Cl3 C43 H43A 109.2 . . ?
Cl2 C43 H43B 109.2 . . ?
Cl3 C43 H43B 109.2 . . ?
H43A C43 H43B 107.9 . . ?
C9 O1 C10 115.5(2) . . ?
C11 O3 C12 119.0(14) . . ?
O3A C12A H12D 109.5 . . ?
O3A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
O3A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C11 O3A C12A 114.3(9) . . ?
C27 O5 C28 115.8(2) . . ?
C29 O7 C30 115.8(2) . . ?
C13 P1 C19 106.97(9) . . ?
C13 P1 C7 108.00(8) . . ?
C19 P1 C7 104.99(9) . . ?
C13 P1 Pd1 120.66(6) . . ?
C19 P1 Pd1 112.78(7) . . ?
C7 P1 Pd1 102.19(6) . . ?
C37 P2 C31 103.74(9) . . ?
C37 P2 C25 108.53(10) . . ?
C31 P2 C25 105.68(9) . . ?
C37 P2 Pd1 113.67(7) . . ?
C31 P2 Pd1 125.24(7) . . ?
C25 P2 Pd1 98.82(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        37.57
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.101
_database_code_depnum_ccdc_archive 'CCDC 991033'
#######################################################################
#
#                 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_I
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H29 O5 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         476.48
_chemical_absolute_configuration ad

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.751(2)
_cell_length_b                   5.8887(8)
_cell_length_c                   19.552(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.361(9)
_cell_angle_gamma                90
_cell_volume                     1204.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1590
_cell_measurement_theta_min      2.4292
_cell_measurement_theta_max      23.3186
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             504

_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.99

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            20068
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.1399
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         31.22
_diffrn_reflns_theta_full        31.22
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       26

_refine_special_details          
;
;

_reflns_number_total             7734
_reflns_number_gt                5156
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0648
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1236
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.990
_refine_ls_number_reflns         7734
_refine_ls_number_parameters     309
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0327P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.477
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Flack x determined using 1521 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.07(10)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 1.3449(4) 1.3698(6) 0.3343(2) 0.0192(8) Uani d . . . 1 . .
H H1 1.2999 1.4903 0.3071 0.023 Uiso calc U . R 1 . .
C C2 1.4739(4) 1.3954(7) 0.3648(2) 0.0238(9) Uani d . . . 1 . .
H H2 1.5174 1.53 0.3572 0.029 Uiso calc U . R 1 . .
C C3 1.5388(4) 1.2229(7) 0.4066(2) 0.0240(9) Uani d . . . 1 . .
H H3 1.6266 1.241 0.4288 0.029 Uiso calc U . R 1 . .
C C4 1.4758(4) 1.0247(6) 0.41587(19) 0.0210(9) Uani d . . . 1 . .
H H4 1.5206 0.9064 0.4443 0.025 Uiso calc U . R 1 . .
C C5 1.3484(4) 0.9981(6) 0.38408(18) 0.0171(8) Uani d . . . 1 . .
H H5 1.3063 0.8604 0.3903 0.021 Uiso calc U . R 1 . .
C C6 1.2800(3) 1.1708(6) 0.34277(18) 0.0137(7) Uani d . . . 1 . .
C C7 1.1433(4) 1.1524(6) 0.30883(18) 0.0138(7) Uani d . . . 1 . .
H H7 1.0986 1.2909 0.2961 0.017 Uiso calc U . R 1 . .
C C8 1.0757(3) 0.9628(6) 0.29410(17) 0.0142(7) Uani d . . . 1 . .
H H8 1.1162 0.8227 0.3097 0.017 Uiso calc U . R 1 . .
C C9 0.9389(3) 0.9580(6) 0.25412(17) 0.0119(7) Uani d . . . 1 . .
H H9 0.8996 1.112 0.2539 0.014 Uiso calc U . R 1 . .
C C10 0.9331(3) 0.8777(6) 0.17771(17) 0.0134(7) Uani d . . . 1 . .
H H10 0.9516 0.7112 0.1788 0.016 Uiso calc U . R 1 . .
C C11 0.8046(4) 0.9181(6) 0.12712(18) 0.0146(7) Uani d . . . 1 . .
C C12 0.6608(4) 0.7583(8) 0.02827(18) 0.0242(8) Uani d . . . 1 . .
H H12A 0.6565 0.895 -0.0017 0.029 Uiso calc U . R 1 . .
H H12B 0.5891 0.7634 0.0522 0.029 Uiso calc U . R 1 . .
C C13 0.6532(4) 0.5463(7) -0.0156(2) 0.0320(11) Uani d . . . 1 . .
H H13A 0.7254 0.5425 -0.0384 0.048 Uiso calc U . R 1 . .
H H13B 0.5728 0.5459 -0.0515 0.048 Uiso calc U . R 1 . .
H H13C 0.6566 0.4126 0.0146 0.048 Uiso calc U . R 1 . .
C C14 1.0365(4) 1.0003(6) 0.14962(18) 0.0146(8) Uani d . . . 1 . .
C C15 1.1221(4) 1.3618(6) 0.1318(2) 0.0190(8) Uani d . . . 1 . .
H H15A 1.2021 1.2726 0.1393 0.023 Uiso calc U . R 1 . .
H H15B 1.1384 1.4986 0.1619 0.023 Uiso calc U . R 1 . .
C C16 1.0802(4) 1.4304(7) 0.0558(2) 0.0283(10) Uani d . . . 1 . .
H H16A 1.0738 1.2952 0.0259 0.042 Uiso calc U . R 1 . .
H H16B 1.1429 1.5357 0.0442 0.042 Uiso calc U . R 1 . .
H H16C 0.9966 1.505 0.0477 0.042 Uiso calc U . R 1 . .
C C17 0.8490(3) 0.8610(6) 0.38147(18) 0.0132(7) Uani d . . . 1 . .
C C18 0.8003(3) 0.7116(6) 0.42400(17) 0.0151(8) Uani d . . . 1 . .
H H18 0.77 0.5667 0.4063 0.018 Uiso calc U . R 1 . .
C C19 0.7955(4) 0.7714(7) 0.49151(18) 0.0198(8) Uani d . . . 1 . .
H H19 0.762 0.6682 0.52 0.024 Uiso calc U . R 1 . .
C C20 0.8398(4) 0.9828(7) 0.51765(19) 0.0189(8) Uani d . . . 1 . .
H H20 0.8382 1.0231 0.5645 0.023 Uiso calc U . R 1 . .
C C21 0.8863(4) 1.1351(6) 0.47577(18) 0.0170(8) Uani d . . . 1 . .
H H21 0.9152 1.2805 0.4936 0.02 Uiso calc U . R 1 . .
C C22 0.8908(3) 1.0754(6) 0.40739(18) 0.0142(7) Uani d . . . 1 . .
H H22 0.9221 1.1805 0.3785 0.017 Uiso calc U . R 1 . .
C C23 0.6889(3) 0.7396(7) 0.24895(16) 0.0130(7) Uani d . . . 1 . .
C C24 0.6458(4) 0.5497(6) 0.20781(18) 0.0179(8) Uani d . . . 1 . .
H H24 0.7037 0.4311 0.204 0.022 Uiso calc U . R 1 . .
C C25 0.5183(4) 0.5332(7) 0.1723(2) 0.0251(9) Uani d . . . 1 . .
H H25 0.4893 0.4041 0.144 0.03 Uiso calc U . R 1 . .
C C26 0.4338(4) 0.7040(7) 0.1783(2) 0.0251(9) Uani d . . . 1 . .
H H26 0.3466 0.6919 0.1541 0.03 Uiso calc U . R 1 . .
C C27 0.4753(4) 0.8921(7) 0.2191(2) 0.0229(9) Uani d . . . 1 . .
H H27 0.4165 1.0092 0.2228 0.028 Uiso calc U . R 1 . .
C C28 0.6023(3) 0.9116(6) 0.25465(18) 0.0173(8) Uani d . . . 1 . .
H H28 0.6303 1.0414 0.2828 0.021 Uiso calc U . R 1 . .
O O1 0.7340(3) 1.0755(4) 0.12799(13) 0.0201(6) Uani d . . . 1 . .
O O2 0.7825(2) 0.7501(5) 0.07970(12) 0.0192(5) Uani d . . . 1 . .
O O3 1.1222(3) 0.9054(5) 0.13114(15) 0.0257(7) Uani d . . . 1 . .
O O4 1.0209(2) 1.2247(4) 0.15027(13) 0.0190(6) Uani d . . . 1 . .
O O5 0.9156(2) 0.5237(4) 0.29903(12) 0.0166(6) Uani d . . . 1 . .
P P1 0.85327(9) 0.75129(15) 0.29610(5) 0.01201(19) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.385(5) ?
C1 C6 . 1.393(5) ?
C1 H1 . 0.95 ?
C2 C3 . 1.386(6) ?
C2 H2 . 0.95 ?
C3 C4 . 1.382(5) ?
C3 H3 . 0.95 ?
C4 C5 . 1.376(5) ?
C4 H4 . 0.95 ?
C5 C6 . 1.398(5) ?
C5 H5 . 0.95 ?
C6 C7 . 1.470(5) ?
C7 C8 . 1.327(5) ?
C7 H7 . 0.95 ?
C8 C9 . 1.498(5) ?
C8 H8 . 0.95 ?
C9 C10 . 1.554(4) ?
C9 P1 . 1.831(3) ?
C9 H9 . 1.0 ?
C10 C11 . 1.520(5) ?
C10 C14 . 1.530(5) ?
C10 H10 . 1.0 ?
C11 O1 . 1.201(4) ?
C11 O2 . 1.339(4) ?
C12 O2 . 1.455(4) ?
C12 C13 . 1.506(6) ?
C12 H12A . 0.99 ?
C12 H12B . 0.99 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C14 O3 . 1.202(4) ?
C14 O4 . 1.332(4) ?
C15 O4 . 1.466(4) ?
C15 C16 . 1.505(5) ?
C15 H15A . 0.99 ?
C15 H15B . 0.99 ?
C16 H16A . 0.98 ?
C16 H16B . 0.98 ?
C16 H16C . 0.98 ?
C17 C18 . 1.393(5) ?
C17 C22 . 1.396(5) ?
C17 P1 . 1.800(4) ?
C18 C19 . 1.379(5) ?
C18 H18 . 0.95 ?
C19 C20 . 1.387(5) ?
C19 H19 . 0.95 ?
C20 C21 . 1.384(5) ?
C20 H20 . 0.95 ?
C21 C22 . 1.394(5) ?
C21 H21 . 0.95 ?
C22 H22 . 0.95 ?
C23 C24 . 1.393(5) ?
C23 C28 . 1.398(5) ?
C23 P1 . 1.795(3) ?
C24 C25 . 1.389(5) ?
C24 H24 . 0.95 ?
C25 C26 . 1.378(5) ?
C25 H25 . 0.95 ?
C26 C27 . 1.378(6) ?
C26 H26 . 0.95 ?
C27 C28 . 1.387(5) ?
C27 H27 . 0.95 ?
C28 H28 . 0.95 ?
O5 P1 . 1.494(2) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 121.3(4) ?
C2 C1 H1 . . 119.4 ?
C6 C1 H1 . . 119.4 ?
C1 C2 C3 . . 119.5(4) ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
C4 C3 C2 . . 120.0(4) ?
C4 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
C5 C4 C3 . . 120.2(4) ?
C5 C4 H4 . . 119.9 ?
C3 C4 H4 . . 119.9 ?
C4 C5 C6 . . 121.0(4) ?
C4 C5 H5 . . 119.5 ?
C6 C5 H5 . . 119.5 ?
C1 C6 C5 . . 118.0(3) ?
C1 C6 C7 . . 119.0(3) ?
C5 C6 C7 . . 123.0(3) ?
C8 C7 C6 . . 126.9(3) ?
C8 C7 H7 . . 116.6 ?
C6 C7 H7 . . 116.6 ?
C7 C8 C9 . . 123.5(3) ?
C7 C8 H8 . . 118.3 ?
C9 C8 H8 . . 118.3 ?
C8 C9 C10 . . 108.9(3) ?
C8 C9 P1 . . 108.3(2) ?
C10 C9 P1 . . 108.4(2) ?
C8 C9 H9 . . 110.4 ?
C10 C9 H9 . . 110.4 ?
P1 C9 H9 . . 110.4 ?
C11 C10 C14 . . 108.6(3) ?
C11 C10 C9 . . 114.0(3) ?
C14 C10 C9 . . 109.3(3) ?
C11 C10 H10 . . 108.3 ?
C14 C10 H10 . . 108.3 ?
C9 C10 H10 . . 108.3 ?
O1 C11 O2 . . 124.6(3) ?
O1 C11 C10 . . 126.4(3) ?
O2 C11 C10 . . 108.9(3) ?
O2 C12 C13 . . 106.7(3) ?
O2 C12 H12A . . 110.4 ?
C13 C12 H12A . . 110.4 ?
O2 C12 H12B . . 110.4 ?
C13 C12 H12B . . 110.4 ?
H12A C12 H12B . . 108.6 ?
C12 C13 H13A . . 109.5 ?
C12 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C12 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
O3 C14 O4 . . 124.8(3) ?
O3 C14 C10 . . 124.0(3) ?
O4 C14 C10 . . 111.1(3) ?
O4 C15 C16 . . 108.8(3) ?
O4 C15 H15A . . 109.9 ?
C16 C15 H15A . . 109.9 ?
O4 C15 H15B . . 109.9 ?
C16 C15 H15B . . 109.9 ?
H15A C15 H15B . . 108.3 ?
C15 C16 H16A . . 109.5 ?
C15 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C15 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C18 C17 C22 . . 119.2(3) ?
C18 C17 P1 . . 114.9(3) ?
C22 C17 P1 . . 125.9(3) ?
C19 C18 C17 . . 120.8(3) ?
C19 C18 H18 . . 119.6 ?
C17 C18 H18 . . 119.6 ?
C18 C19 C20 . . 119.8(3) ?
C18 C19 H19 . . 120.1 ?
C20 C19 H19 . . 120.1 ?
C21 C20 C19 . . 120.2(3) ?
C21 C20 H20 . . 119.9 ?
C19 C20 H20 . . 119.9 ?
C20 C21 C22 . . 120.1(4) ?
C20 C21 H21 . . 119.9 ?
C22 C21 H21 . . 119.9 ?
C21 C22 C17 . . 119.8(3) ?
C21 C22 H22 . . 120.1 ?
C17 C22 H22 . . 120.1 ?
C24 C23 C28 . . 119.2(3) ?
C24 C23 P1 . . 119.0(3) ?
C28 C23 P1 . . 121.7(3) ?
C25 C24 C23 . . 120.2(4) ?
C25 C24 H24 . . 119.9 ?
C23 C24 H24 . . 119.9 ?
C26 C25 C24 . . 120.0(4) ?
C26 C25 H25 . . 120.0 ?
C24 C25 H25 . . 120.0 ?
C25 C26 C27 . . 120.3(4) ?
C25 C26 H26 . . 119.8 ?
C27 C26 H26 . . 119.8 ?
C26 C27 C28 . . 120.4(4) ?
C26 C27 H27 . . 119.8 ?
C28 C27 H27 . . 119.8 ?
C27 C28 C23 . . 119.8(4) ?
C27 C28 H28 . . 120.1 ?
C23 C28 H28 . . 120.1 ?
C11 O2 C12 . . 116.2(3) ?
C14 O4 C15 . . 116.2(3) ?
O5 P1 C23 . . 111.40(17) ?
O5 P1 C17 . . 113.18(15) ?
C23 P1 C17 . . 104.91(16) ?
O5 P1 C9 . . 110.24(15) ?
C23 P1 C9 . . 109.43(16) ?
C17 P1 C9 . . 107.47(16) ?

_database_code_depnum_ccdc_archive 'CCDC 991034'
#######################################################################
#
#                 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_I
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H29 O5 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         476.48

_chemical_melting_point          ?

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

_cell_length_a                   5.6363(4)
_cell_length_b                   12.4972(11)
_cell_length_c                   18.9559(17)
_cell_angle_alpha                103.051(6)
_cell_angle_beta                 96.273(5)
_cell_angle_gamma                102.019(5)
_cell_volume                     1254.98(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4246
_cell_measurement_theta_min      2.2361
_cell_measurement_theta_max      29.1179
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             504

_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_T_max  0.97

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            38041
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         31.21
_diffrn_reflns_theta_full        31.21
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27

_refine_special_details          
;
;

_reflns_number_total             8090
_reflns_number_gt                5837
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1272
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.003
_refine_ls_number_reflns         8090
_refine_ls_number_parameters     489
_refine_ls_number_restraints     925
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0580P)²+0.1067P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.6254(2) 0.15793(12) 0.26763(8) 0.0184(3) Uani d . . . 1.0 . .
H H1 0.536 0.2145 0.2788 0.022 Uiso calc U . R 1.0 . .
C C2 0.5523(2) 0.05648(12) 0.28632(8) 0.0199(3) Uani d . . . 1.0 . .
H H2 0.4139 0.0444 0.3105 0.024 Uiso calc U . R 1.0 . .
C C3 0.6788(3) -0.02750(12) 0.27008(8) 0.0218(3) Uani d . . . 1.0 . .
H H3 0.6272 -0.0973 0.2825 0.026 Uiso calc U . R 1.0 . .
C C4 0.8821(3) -0.00825(13) 0.23537(8) 0.0230(3) Uani d . . . 1.0 . .
H H4 0.971 -0.065 0.2243 0.028 Uiso calc U . R 1.0 . .
C C5 0.9565(2) 0.09343(12) 0.21676(7) 0.0170(3) Uani d . . . 1.0 . .
H H5 1.0959 0.1055 0.193 0.02 Uiso calc U . R 1.0 . .
C C6 0.8294(2) 0.17766(11) 0.23250(7) 0.0130(2) Uani d . . . 1.0 . .
C C7 0.9219(2) 0.29047(11) 0.21528(7) 0.0132(2) Uani d . . . 1.0 . .
H H7 1.0732 0.2871 0.1926 0.016 Uiso calc U . R 1.0 . .
C C8 0.9903(2) 0.38682(11) 0.28421(7) 0.0148(3) Uani d . . . 1.0 . .
H H8 0.8683 0.3994 0.3138 0.018 Uiso calc U . R 1.0 . .
C C9 1.2137(2) 0.45408(11) 0.30475(7) 0.0171(3) Uani d . . . 1.0 . .
H H9 1.3372 0.4397 0.2761 0.02 Uiso calc U . R 1.0 . .
C C10 1.2802(2) 0.55280(11) 0.37181(7) 0.0156(3) Uani d . . D 1.0 . .
H H10 1.148 0.545 0.4028 0.019 Uiso calc U P R 0.453(3) A 1
H H10A 1.1479 0.5452 0.4027 0.019 Uiso calc U P R 0.254(3) A 2
H H10B 1.1508 0.5398 0.4031 0.019 Uiso calc U P R 0.293(3) A 3
C C14 1.5247(3) 0.56065(11) 0.41776(7) 0.0170(3) Uani d . . . 1.0 . .
C C15 1.8175(3) 0.67894(13) 0.52010(8) 0.0264(3) Uani d . . . 1.0 . .
H H15A 1.9608 0.6918 0.4945 0.032 Uiso calc U . R 1.0 . .
H H15B 1.8202 0.6134 0.541 0.032 Uiso calc U . R 1.0 . .
C C16 1.8252(4) 0.78153(18) 0.57908(10) 0.0528(6) Uani d . . . 1.0 . .
H H16A 1.8131 0.8446 0.5572 0.079 Uiso calc U . R 1.0 . .
H H16B 1.9804 0.8014 0.6133 0.079 Uiso calc U . R 1.0 . .
H H16C 1.6872 0.7661 0.6055 0.079 Uiso calc U . R 1.0 . .
C C11 1.295(2) 0.6596(8) 0.3473(7) 0.021(2) Uani d U P D 0.453(3) A 1
C C12 1.0509(7) 0.7882(3) 0.3295(2) 0.0262(8) Uani d U P D 0.453(3) A 1
H H12A 0.8782 0.7781 0.3068 0.031 Uiso calc U P R 0.453(3) A 1
H H12B 1.1575 0.8008 0.2924 0.031 Uiso calc U P R 0.453(3) A 1
C C13 1.1208(13) 0.8881(4) 0.3948(3) 0.0480(14) Uani d U P D 0.453(3) A 1
H H13A 1.0241 0.8726 0.4329 0.072 Uiso calc U P R 0.453(3) A 1
H H13B 1.0878 0.9548 0.3804 0.072 Uiso calc U P R 0.453(3) A 1
H H13C 1.2962 0.9023 0.414 0.072 Uiso calc U P R 0.453(3) A 1
O O1 1.461(3) 0.7084(18) 0.3232(8) 0.024(2) Uani d U P D 0.453(3) A 1
O O2 1.0793(8) 0.6875(3) 0.35273(19) 0.0232(7) Uani d U P D 0.453(3) A 1
C C11A 1.305(5) 0.6654(16) 0.3495(17) 0.012(3) Uani d U P D 0.254(3) A 2
C C12A 1.176(3) 0.8387(12) 0.3724(9) 0.029(2) Uani d U P D 0.254(3) A 2
H H12C 1.115 0.8312 0.3201 0.034 Uiso calc U P R 0.254(3) A 2
H H12D 1.3468 0.8858 0.385 0.034 Uiso calc U P R 0.254(3) A 2
C C13A 1.0124(14) 0.8926(6) 0.4210(4) 0.0290(15) Uani d U P D 0.254(3) A 2
H H13D 0.8467 0.8427 0.4102 0.043 Uiso calc U P R 0.254(3) A 2
H H13E 1.0042 0.9657 0.4115 0.043 Uiso calc U P R 0.254(3) A 2
H H13F 1.081 0.9041 0.4727 0.043 Uiso calc U P R 0.254(3) A 2
O O1A 1.445(7) 0.696(2) 0.3101(18) 0.016(4) Uani d U P D 0.254(3) A 2
O O2A 1.168(2) 0.7272(11) 0.3855(10) 0.0188(19) Uani d U P D 0.254(3) A 2
C C11B 1.274(5) 0.6655(15) 0.3516(15) 0.013(3) Uani d U P D 0.293(3) A 3
C C12B 1.129(3) 0.8338(11) 0.3762(8) 0.035(2) Uani d U P D 0.293(3) A 3
H H12E 0.9687 0.8529 0.3807 0.042 Uiso calc U P R 0.293(3) A 3
H H12F 1.1701 0.8408 0.3277 0.042 Uiso calc U P R 0.293(3) A 3
C C13B 1.3259(16) 0.9138(5) 0.4366(4) 0.0508(19) Uani d U P D 0.293(3) A 3
H H13G 1.2961 0.8993 0.4839 0.076 Uiso calc U P R 0.293(3) A 3
H H13H 1.3216 0.9921 0.4375 0.076 Uiso calc U P R 0.293(3) A 3
H H13I 1.4875 0.9019 0.4275 0.076 Uiso calc U P R 0.293(3) A 3
O O1B 1.410(5) 0.702(3) 0.3123(18) 0.021(3) Uani d U P D 0.293(3) A 3
O O2B 1.115(2) 0.7183(10) 0.3823(10) 0.022(2) Uani d U P D 0.293(3) A 3
C C17 0.6746(6) 0.2260(3) 0.05676(12) 0.0119(13) Uani d U P DG 0.502(5) B 1
C C18 0.4999(5) 0.2344(2) 0.00183(14) 0.0176(7) Uani d U P DG 0.502(5) B 1
H H18 0.4067 0.2896 0.012 0.021 Uiso calc U P R 0.502(5) B 1
C C19 0.4617(5) 0.1619(3) -0.06797(13) 0.0189(7) Uani d U P DG 0.502(5) B 1
H H19 0.3424 0.1676 -0.1055 0.023 Uiso calc U P R 0.502(5) B 1
C C20 0.5981(6) 0.0811(2) -0.08283(14) 0.0173(12) Uani d U P DG 0.502(5) B 1
H H20 0.572 0.0316 -0.1305 0.021 Uiso calc U P R 0.502(5) B 1
C C21 0.7728(6) 0.0728(2) -0.02790(18) 0.0160(8) Uani d U P DG 0.502(5) B 1
H H21 0.866 0.0176 -0.0381 0.019 Uiso calc U P R 0.502(5) B 1
C C22 0.8110(6) 0.1452(3) 0.04190(16) 0.0175(9) Uani d U P DG 0.502(5) B 1
H H22 0.9303 0.1395 0.0795 0.021 Uiso calc U P R 0.502(5) B 1
C C23 0.8231(6) 0.46207(16) 0.13914(18) 0.0156(17) Uani d U P DG 0.502(5) B 1
C C24 0.9900(6) 0.4829(2) 0.09216(17) 0.0251(8) Uani d U P DG 0.502(5) B 1
H H24 1.0373 0.4217 0.062 0.03 Uiso calc U P R 0.502(5) B 1
C C25 1.0879(6) 0.5932(2) 0.08924(18) 0.0315(10) Uani d U P DG 0.502(5) B 1
H H25 1.202 0.6074 0.0571 0.038 Uiso calc U P R 0.502(5) B 1
C C26 1.0187(6) 0.68270(19) 0.13331(19) 0.0299(14) Uani d U P DG 0.502(5) B 1
H H26 1.0856 0.7581 0.1313 0.036 Uiso calc U P R 0.502(5) B 1
C C27 0.8518(6) 0.66192(18) 0.18030(18) 0.0286(8) Uani d U P DG 0.502(5) B 1
H H27 0.8045 0.7231 0.2104 0.034 Uiso calc U P R 0.502(5) B 1
C C28 0.7540(5) 0.5516(2) 0.18322(17) 0.0211(7) Uani d U P DG 0.502(5) B 1
H H28 0.6399 0.5374 0.2153 0.025 Uiso calc U P R 0.502(5) B 1
C C17A 0.6816(8) 0.2226(4) 0.0656(3) 0.0133(11) Uani d U P D 0.498(5) B 2
C C18A 0.4571(6) 0.1933(3) 0.01869(18) 0.0193(7) Uani d U P D 0.498(5) B 2
H H18A 0.3249 0.224 0.0341 0.023 Uiso calc U P R 0.498(5) B 2
C C19A 0.4249(6) 0.1199(3) -0.05029(19) 0.0235(8) Uani d U P D 0.498(5) B 2
H H19A 0.2715 0.1013 -0.082 0.028 Uiso calc U P R 0.498(5) B 2
C C20A 0.6131(9) 0.0736(4) -0.0732(3) 0.0194(10) Uani d U P D 0.498(5) B 2
H H20A 0.5876 0.0201 -0.1194 0.023 Uiso calc U P R 0.498(5) B 2
C C21A 0.8405(7) 0.1058(4) -0.0282(2) 0.0187(8) Uani d U P D 0.498(5) B 2
H H21A 0.974 0.0777 -0.0449 0.022 Uiso calc U P R 0.498(5) B 2
C C22A 0.8744(7) 0.1788(3) 0.0411(2) 0.0146(8) Uani d U P D 0.498(5) B 2
H H22A 1.0298 0.199 0.072 0.018 Uiso calc U P R 0.498(5) B 2
C C23A 0.8280(8) 0.4565(3) 0.1418(2) 0.0140(15) Uani d U P D 0.498(5) B 2
C C24A 1.0632(6) 0.4877(3) 0.1246(2) 0.0203(7) Uani d U P D 0.498(5) B 2
H H24A 1.1652 0.4356 0.1201 0.024 Uiso calc U P R 0.498(5) B 2
C C25A 1.1477(7) 0.5937(3) 0.1140(2) 0.0244(8) Uani d U P D 0.498(5) B 2
H H25A 1.3094 0.615 0.1036 0.029 Uiso calc U P R 0.498(5) B 2
C C26A 1.0001(10) 0.6688(4) 0.1185(4) 0.0326(12) Uani d U P D 0.498(5) B 2
H H26A 1.0581 0.7406 0.1094 0.039 Uiso calc U P R 0.498(5) B 2
C C27A 0.7673(7) 0.6406(3) 0.1363(3) 0.0341(10) Uani d U P D 0.498(5) B 2
H H27A 0.667 0.6933 0.1405 0.041 Uiso calc U P R 0.498(5) B 2
C C28A 0.6814(7) 0.5341(3) 0.1480(3) 0.0259(8) Uani d U P D 0.498(5) B 2
H H28A 0.5219 0.5144 0.1603 0.031 Uiso calc U P R 0.498(5) B 2
O O3 1.6391(2) 0.48925(9) 0.41058(6) 0.0279(3) Uani d . . . 1.0 . .
O O4 1.58977(19) 0.65806(8) 0.46937(5) 0.0243(2) Uani d . . . 1.0 . .
O O5 0.44835(16) 0.31189(8) 0.17184(5) 0.0174(2) Uani d . . . 1.0 . .
P P1 0.69558(6) 0.31981(3) 0.14976(2) 0.01308(9) Uani d . . D 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.3855(19) ?
C1 C6 . 1.3962(18) ?
C1 H1 . 0.95 ?
C2 C3 . 1.385(2) ?
C2 H2 . 0.95 ?
C3 C4 . 1.387(2) ?
C3 H3 . 0.95 ?
C4 C5 . 1.388(2) ?
C4 H4 . 0.95 ?
C5 C6 . 1.3889(18) ?
C5 H5 . 0.95 ?
C6 C7 . 1.5181(18) ?
C7 C8 . 1.5138(18) ?
C7 P1 . 1.8326(13) ?
C7 H7 . 1.0 ?
C8 C9 . 1.3220(19) ?
C8 H8 . 0.95 ?
C9 C10 . 1.5078(18) ?
C9 H9 . 0.95 ?
C10 C11 . 1.499(9) ?
C10 C14 . 1.5200(19) ?
C10 C11A . 1.542(11) ?
C10 C11B . 1.547(11) ?
C10 H10 . 1.0 ?
C10 H10A . 1.0 ?
C10 H10B . 1.0 ?
C14 O3 . 1.1975(16) ?
C14 O4 . 1.3308(16) ?
C15 O4 . 1.4552(17) ?
C15 C16 . 1.488(2) ?
C15 H15A . 0.99 ?
C15 H15B . 0.99 ?
C16 H16A . 0.98 ?
C16 H16B . 0.98 ?
C16 H16C . 0.98 ?
C11 O1 . 1.197(9) ?
C11 O2 . 1.342(9) ?
C12 O2 . 1.458(4) ?
C12 C13 . 1.496(6) ?
C12 H12A . 0.99 ?
C12 H12B . 0.99 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C11A O1A . 1.207(12) ?
C11A O2A . 1.336(12) ?
C12A O2A . 1.462(10) ?
C12A C13A . 1.523(13) ?
C12A H12C . 0.99 ?
C12A H12D . 0.99 ?
C13A H13D . 0.98 ?
C13A H13E . 0.98 ?
C13A H13F . 0.98 ?
C11B O1B . 1.215(12) ?
C11B O2B . 1.332(11) ?
C12B O2B . 1.460(10) ?
C12B C13B . 1.512(14) ?
C12B H12E . 0.99 ?
C12B H12F . 0.99 ?
C13B H13G . 0.98 ?
C13B H13H . 0.98 ?
C13B H13I . 0.98 ?
C17 C18 . 1.39 ?
C17 C22 . 1.39 ?
C17 P1 . 1.860(2) ?
C18 C19 . 1.39 ?
C18 H18 . 0.95 ?
C19 C20 . 1.39 ?
C19 H19 . 0.95 ?
C20 C21 . 1.39 ?
C20 H20 . 0.95 ?
C21 C22 . 1.39 ?
C21 H21 . 0.95 ?
C22 H22 . 0.95 ?
C23 C24 . 1.39 ?
C23 C28 . 1.39 ?
C23 P1 . 1.8382(19) ?
C24 C25 . 1.39 ?
C24 H24 . 0.95 ?
C25 C26 . 1.39 ?
C25 H25 . 0.95 ?
C26 C27 . 1.39 ?
C26 H26 . 0.95 ?
C27 C28 . 1.39 ?
C27 H27 . 0.95 ?
C28 H28 . 0.95 ?
C17A C22A . 1.393(4) ?
C17A C18A . 1.393(5) ?
C17A P1 . 1.756(4) ?
C18A C19A . 1.386(4) ?
C18A H18A . 0.95 ?
C19A C20A . 1.375(5) ?
C19A H19A . 0.95 ?
C20A C21A . 1.387(5) ?
C20A H20A . 0.95 ?
C21A C22A . 1.388(4) ?
C21A H21A . 0.95 ?
C22A H22A . 0.95 ?
C23A C28A . 1.394(5) ?
C23A C24A . 1.398(5) ?
C23A P1 . 1.763(4) ?
C24A C25A . 1.378(4) ?
C24A H24A . 0.95 ?
C25A C26A . 1.373(5) ?
C25A H25A . 0.95 ?
C26A C27A . 1.385(5) ?
C26A H26A . 0.95 ?
C27A C28A . 1.393(4) ?
C27A H27A . 0.95 ?
C28A H28A . 0.95 ?
O5 P1 . 1.4884(9) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 120.51(13) ?
C2 C1 H1 . . 119.7 ?
C6 C1 H1 . . 119.7 ?
C3 C2 C1 . . 120.73(13) ?
C3 C2 H2 . . 119.6 ?
C1 C2 H2 . . 119.6 ?
C2 C3 C4 . . 119.02(13) ?
C2 C3 H3 . . 120.5 ?
C4 C3 H3 . . 120.5 ?
C3 C4 C5 . . 120.45(13) ?
C3 C4 H4 . . 119.8 ?
C5 C4 H4 . . 119.8 ?
C4 C5 C6 . . 120.77(13) ?
C4 C5 H5 . . 119.6 ?
C6 C5 H5 . . 119.6 ?
C5 C6 C1 . . 118.51(12) ?
C5 C6 C7 . . 119.84(11) ?
C1 C6 C7 . . 121.56(11) ?
C8 C7 C6 . . 111.44(10) ?
C8 C7 P1 . . 109.35(9) ?
C6 C7 P1 . . 111.94(9) ?
C8 C7 H7 . . 108.0 ?
C6 C7 H7 . . 108.0 ?
P1 C7 H7 . . 108.0 ?
C9 C8 C7 . . 122.43(12) ?
C9 C8 H8 . . 118.8 ?
C7 C8 H8 . . 118.8 ?
C8 C9 C10 . . 122.61(12) ?
C8 C9 H9 . . 118.7 ?
C10 C9 H9 . . 118.7 ?
C11 C10 C9 . . 108.5(5) ?
C11 C10 C14 . . 108.8(5) ?
C9 C10 C14 . . 112.72(11) ?
C9 C10 C11A . . 110.6(12) ?
C14 C10 C11A . . 106.4(13) ?
C9 C10 C11B . . 111.6(11) ?
C14 C10 C11B . . 111.3(12) ?
C11 C10 H10 . . 108.9 ?
C9 C10 H10 . . 108.9 ?
C14 C10 H10 . . 108.9 ?
C9 C10 H10A . . 109.0 ?
C14 C10 H10A . . 109.0 ?
C11A C10 H10A . . 109.0 ?
C9 C10 H10B . . 107.0 ?
C14 C10 H10B . . 107.0 ?
C11B C10 H10B . . 107.0 ?
O3 C14 O4 . . 124.70(13) ?
O3 C14 C10 . . 125.72(12) ?
O4 C14 C10 . . 109.54(11) ?
O4 C15 C16 . . 106.49(14) ?
O4 C15 H15A . . 110.4 ?
C16 C15 H15A . . 110.4 ?
O4 C15 H15B . . 110.4 ?
C16 C15 H15B . . 110.4 ?
H15A C15 H15B . . 108.6 ?
C15 C16 H16A . . 109.5 ?
C15 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C15 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
O1 C11 O2 . . 125.4(13) ?
O1 C11 C10 . . 127.4(13) ?
O2 C11 C10 . . 107.1(7) ?
O2 C12 C13 . . 109.1(3) ?
O2 C12 H12A . . 109.9 ?
C13 C12 H12A . . 109.9 ?
O2 C12 H12B . . 109.9 ?
C13 C12 H12B . . 109.9 ?
H12A C12 H12B . . 108.3 ?
C12 C13 H13A . . 109.5 ?
C12 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C12 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C11 O2 C12 . . 116.3(5) ?
O1A C11A O2A . . 125.7(16) ?
O1A C11A C10 . . 124.0(17) ?
O2A C11A C10 . . 110.1(12) ?
O2A C12A C13A . . 106.8(11) ?
O2A C12A H12C . . 110.4 ?
C13A C12A H12C . . 110.4 ?
O2A C12A H12D . . 110.4 ?
C13A C12A H12D . . 110.4 ?
H12C C12A H12D . . 108.6 ?
C12A C13A H13D . . 109.5 ?
C12A C13A H13E . . 109.5 ?
H13D C13A H13E . . 109.5 ?
C12A C13A H13F . . 109.5 ?
H13D C13A H13F . . 109.5 ?
H13E C13A H13F . . 109.5 ?
C11A O2A C12A . . 117.1(11) ?
O1B C11B O2B . . 124.3(16) ?
O1B C11B C10 . . 121.6(18) ?
O2B C11B C10 . . 114.1(12) ?
O2B C12B C13B . . 108.7(11) ?
O2B C12B H12E . . 109.9 ?
C13B C12B H12E . . 109.9 ?
O2B C12B H12F . . 109.9 ?
C13B C12B H12F . . 109.9 ?
H12E C12B H12F . . 108.3 ?
C12B C13B H13G . . 109.5 ?
C12B C13B H13H . . 109.5 ?
H13G C13B H13H . . 109.5 ?
C12B C13B H13I . . 109.5 ?
H13G C13B H13I . . 109.5 ?
H13H C13B H13I . . 109.5 ?
C11B O2B C12B . . 117.0(10) ?
C18 C17 C22 . . 120.0 ?
C18 C17 P1 . . 116.55(15) ?
C22 C17 P1 . . 123.31(15) ?
C19 C18 C17 . . 120.0 ?
C19 C18 H18 . . 120.0 ?
C17 C18 H18 . . 120.0 ?
C18 C19 C20 . . 120.0 ?
C18 C19 H19 . . 120.0 ?
C20 C19 H19 . . 120.0 ?
C19 C20 C21 . . 120.0 ?
C19 C20 H20 . . 120.0 ?
C21 C20 H20 . . 120.0 ?
C22 C21 C20 . . 120.0 ?
C22 C21 H21 . . 120.0 ?
C20 C21 H21 . . 120.0 ?
C21 C22 C17 . . 120.0 ?
C21 C22 H22 . . 120.0 ?
C17 C22 H22 . . 120.0 ?
C24 C23 C28 . . 120.0 ?
C24 C23 P1 . . 122.96(14) ?
C28 C23 P1 . . 116.97(14) ?
C23 C24 C25 . . 120.0 ?
C23 C24 H24 . . 120.0 ?
C25 C24 H24 . . 120.0 ?
C26 C25 C24 . . 120.0 ?
C26 C25 H25 . . 120.0 ?
C24 C25 H25 . . 120.0 ?
C25 C26 C27 . . 120.0 ?
C25 C26 H26 . . 120.0 ?
C27 C26 H26 . . 120.0 ?
C28 C27 C26 . . 120.0 ?
C28 C27 H27 . . 120.0 ?
C26 C27 H27 . . 120.0 ?
C27 C28 C23 . . 120.0 ?
C27 C28 H28 . . 120.0 ?
C23 C28 H28 . . 120.0 ?
C22A C17A C18A . . 118.6(3) ?
C22A C17A P1 . . 126.3(3) ?
C18A C17A P1 . . 115.0(3) ?
C19A C18A C17A . . 120.6(3) ?
C19A C18A H18A . . 119.7 ?
C17A C18A H18A . . 119.7 ?
C20A C19A C18A . . 120.6(3) ?
C20A C19A H19A . . 119.7 ?
C18A C19A H19A . . 119.7 ?
C19A C20A C21A . . 119.3(3) ?
C19A C20A H20A . . 120.3 ?
C21A C20A H20A . . 120.3 ?
C20A C21A C22A . . 120.5(3) ?
C20A C21A H21A . . 119.8 ?
C22A C21A H21A . . 119.8 ?
C21A C22A C17A . . 120.3(3) ?
C21A C22A H22A . . 119.9 ?
C17A C22A H22A . . 119.9 ?
C28A C23A C24A . . 118.9(3) ?
C28A C23A P1 . . 117.4(3) ?
C24A C23A P1 . . 123.5(3) ?
C25A C24A C23A . . 120.2(3) ?
C25A C24A H24A . . 119.9 ?
C23A C24A H24A . . 119.9 ?
C26A C25A C24A . . 120.5(3) ?
C26A C25A H25A . . 119.7 ?
C24A C25A H25A . . 119.7 ?
C25A C26A C27A . . 120.5(3) ?
C25A C26A H26A . . 119.8 ?
C27A C26A H26A . . 119.8 ?
C26A C27A C28A . . 119.5(3) ?
C26A C27A H27A . . 120.3 ?
C28A C27A H27A . . 120.3 ?
C27A C28A C23A . . 120.4(3) ?
C27A C28A H28A . . 119.8 ?
C23A C28A H28A . . 119.8 ?
C14 O4 C15 . . 117.22(11) ?
O5 P1 C17A . . 111.35(15) ?
O5 P1 C23A . . 112.01(14) ?
C17A P1 C23A . . 108.3(2) ?
O5 P1 C7 . . 113.97(6) ?
C17A P1 C7 . . 105.83(16) ?
C23A P1 C7 . . 104.89(17) ?
O5 P1 C23 . . 110.70(10) ?
C7 P1 C23 . . 107.04(13) ?
O5 P1 C17 . . 110.97(11) ?
C7 P1 C17 . . 109.97(9) ?
C23 P1 C17 . . 103.61(14) ?

_database_code_depnum_ccdc_archive 'CCDC 991035'
