Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Yoshitane Imai'
_publ_contact_author_email       Y-IMAI@APCH.KINDAI.AC.JP

_publ_section_title              
;
Formation of Supramolecular Host System with Multiple
Chiral Points (Central, Axial, and Helical) by using
(1R,2S)-2-Amino-1,2-diphenylethanol
;
loop_
_publ_author_name
'Yoshitane Imai'
'Reiko Kuroda'
'Yoshio Matsubara'
'Hideki Matsuno'
'Katuzo Murata'
'Tomohiro Sato'

# Attachment 'IMAI717.CIF'

data_imai717_1
_database_code_depnum_ccdc_archive 'CCDC 671745'
#data_im7627a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H34 N O6 P'
_chemical_formula_weight         607.61
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   8.6165(4)
_cell_length_b                   14.8416(7)
_cell_length_c                   24.3940(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3119.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    6441
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      27.92

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9414
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      130(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  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19549
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.92
_reflns_number_total             7050
_reflns_number_gt                6541
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+1.2178P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(9)
_refine_ls_number_reflns         7050
_refine_ls_number_parameters     401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.0991
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
C1 C 0.3533(2) 0.28644(13) 0.75962(7) 0.0163(4) Uani 1 1 d . . .
C2 C 0.3307(2) 0.20809(13) 0.78845(8) 0.0165(4) Uani 1 1 d . . .
C3 C 0.4054(2) 0.12657(13) 0.77548(8) 0.0207(4) Uani 1 1 d . . .
H3 H 0.3845 0.0736 0.7960 0.025 Uiso 1 1 calc R . .
C4 C 0.5081(3) 0.12464(13) 0.73296(9) 0.0239(4) Uani 1 1 d . . .
H4 H 0.5559 0.0694 0.7229 0.029 Uiso 1 1 calc R . .
C5 C 0.6571(3) 0.20421(16) 0.66122(9) 0.0284(5) Uani 1 1 d . . .
H5 H 0.7049 0.1492 0.6507 0.034 Uiso 1 1 calc R . .
C6 C 0.6976(3) 0.28165(16) 0.63547(9) 0.0323(5) Uani 1 1 d . . .
H6 H 0.7739 0.2804 0.6074 0.039 Uiso 1 1 calc R . .
C7 C 0.6277(3) 0.36383(15) 0.65002(9) 0.0282(5) Uani 1 1 d . . .
H7 H 0.6583 0.4179 0.6322 0.034 Uiso 1 1 calc R . .
C8 C 0.5159(2) 0.36598(14) 0.68966(8) 0.0214(4) Uani 1 1 d . . .
H8 H 0.4685 0.4217 0.6989 0.026 Uiso 1 1 calc R . .
C9 C 0.4692(2) 0.28603(13) 0.71728(8) 0.0177(4) Uani 1 1 d . . .
C10 C 0.5442(2) 0.20411(14) 0.70364(8) 0.0216(4) Uani 1 1 d . . .
C11 C 0.2607(2) 0.36773(12) 0.77375(7) 0.0154(4) Uani 1 1 d . . .
C12 C 0.2516(2) 0.39581(12) 0.82743(7) 0.0161(4) Uani 1 1 d . . .
C13 C 0.1628(2) 0.46981(13) 0.84429(8) 0.0201(4) Uani 1 1 d . . .
H13 H 0.1576 0.4858 0.8820 0.024 Uiso 1 1 calc R . .
C14 C 0.0839(2) 0.51863(14) 0.80613(9) 0.0219(4) Uani 1 1 d . . .
H14 H 0.0272 0.5704 0.8172 0.026 Uiso 1 1 calc R . .
C15 C -0.0014(3) 0.54147(15) 0.71078(9) 0.0253(4) Uani 1 1 d . . .
H15 H -0.0546 0.5948 0.7213 0.030 Uiso 1 1 calc R . .
C16 C -0.0101(3) 0.51297(15) 0.65790(9) 0.0268(5) Uani 1 1 d . . .
H16 H -0.0685 0.5462 0.6318 0.032 Uiso 1 1 calc R . .
C17 C 0.0681(3) 0.43377(16) 0.64224(9) 0.0263(5) Uani 1 1 d . . .
H17 H 0.0603 0.4131 0.6055 0.032 Uiso 1 1 calc R . .
C18 C 0.1546(2) 0.38648(14) 0.67880(8) 0.0207(4) Uani 1 1 d . . .
H18 H 0.2058 0.3331 0.6672 0.025 Uiso 1 1 calc R . .
C19 C 0.1697(2) 0.41532(12) 0.73389(8) 0.0162(4) Uani 1 1 d . . .
C20 C 0.0852(2) 0.49339(13) 0.75046(8) 0.0188(4) Uani 1 1 d . . .
O1 O 0.22247(15) 0.20575(9) 0.83107(5) 0.0161(3) Uani 1 1 d . . .
O2 O 0.33499(16) 0.34881(9) 0.86733(5) 0.0166(3) Uani 1 1 d . . .
O3 O 0.11275(16) 0.26698(9) 0.91694(5) 0.0204(3) Uani 1 1 d . . .
O4 O 0.38883(16) 0.20806(9) 0.91811(6) 0.0195(3) Uani 1 1 d . . .
P P 0.26256(5) 0.25516(3) 0.888067(19) 0.01504(10) Uani 1 1 d . . .
C31 C 0.2410(3) -0.04803(13) 1.03088(8) 0.0235(4) Uani 1 1 d . . .
C32 C 0.1929(5) -0.11666(17) 0.99674(10) 0.0525(9) Uani 1 1 d . . .
H32 H 0.1690 -0.1038 0.9595 0.063 Uiso 1 1 calc R . .
C33 C 0.1790(6) -0.20389(18) 1.01595(11) 0.0752(13) Uani 1 1 d . . .
H33 H 0.1441 -0.2503 0.9922 0.090 Uiso 1 1 calc R . .
C34 C 0.2161(5) -0.22354(18) 1.06980(11) 0.0650(11) Uani 1 1 d . . .
H34 H 0.2076 -0.2836 1.0830 0.078 Uiso 1 1 calc R . .
C35 C 0.2655(4) -0.15550(16) 1.10433(10) 0.0432(7) Uani 1 1 d . . .
H35 H 0.2927 -0.1688 1.1412 0.052 Uiso 1 1 calc R . .
C36 C 0.2754(3) -0.06769(15) 1.08506(9) 0.0302(5) Uani 1 1 d . . .
H36 H 0.3060 -0.0207 1.1092 0.036 Uiso 1 1 calc R . .
C37 C 0.2390(2) 0.04890(12) 1.01179(7) 0.0183(4) Uani 1 1 d . . .
H37 H 0.3321 0.0805 1.0270 0.022 Uiso 1 1 calc R . .
O38 O 0.24428(17) 0.05310(9) 0.95379(5) 0.0200(3) Uani 1 1 d . . .
H38 H 0.2954 0.0986 0.9441 0.030 Uiso 1 1 calc R . .
C39 C -0.0604(2) 0.06168(14) 1.01012(8) 0.0194(4) Uani 1 1 d . . .
C40 C -0.1302(3) -0.01382(15) 1.03347(9) 0.0286(5) Uani 1 1 d . . .
H40 H -0.0809 -0.0436 1.0632 0.034 Uiso 1 1 calc R . .
C41 C -0.2701(3) -0.04599(16) 1.01391(10) 0.0363(6) Uani 1 1 d . . .
H41 H -0.3150 -0.0982 1.0300 0.044 Uiso 1 1 calc R . .
C42 C -0.3452(3) -0.00326(17) 0.97142(10) 0.0341(6) Uani 1 1 d . . .
H42 H -0.4426 -0.0248 0.9587 0.041 Uiso 1 1 calc R . .
C43 C -0.2772(3) 0.07127(16) 0.94756(10) 0.0307(5) Uani 1 1 d . . .
H43 H -0.3275 0.1009 0.9180 0.037 Uiso 1 1 calc R . .
C44 C -0.1353(3) 0.10318(14) 0.96665(9) 0.0248(4) Uani 1 1 d . . .
H44 H -0.0891 0.1541 0.9496 0.030 Uiso 1 1 calc R . .
C45 C 0.0909(2) 0.09570(13) 1.03379(8) 0.0174(4) Uani 1 1 d . . .
H45 H 0.0872 0.0849 1.0742 0.021 Uiso 1 1 calc R . .
N36 N 0.10857(19) 0.19514(10) 1.02543(7) 0.0164(3) Uani 1 1 d . . .
H36A H 0.1198 0.2069 0.9890 0.025 Uiso 1 1 calc R . .
H36B H 0.1939 0.2149 1.0438 0.025 Uiso 1 1 calc R . .
H36C H 0.0228 0.2239 1.0383 0.025 Uiso 1 1 calc R . .
O51 O -0.18492(17) 0.29765(12) 0.89016(6) 0.0295(4) Uani 1 1 d . . .
H51 H -0.0893 0.2896 0.8948 0.044 Uiso 1 1 calc R . .
C51 C -0.2311(3) 0.25932(17) 0.83876(9) 0.0334(5) Uani 1 1 d . . .
H51A H -0.3457 0.2603 0.8361 0.040 Uiso 1 1 calc R . .
H51B H -0.1970 0.1957 0.8372 0.040 Uiso 1 1 calc R . .
C52 C -0.1642(3) 0.3090(3) 0.79162(11) 0.0569(9) Uani 1 1 d . . .
H52A H -0.2023 0.3712 0.7919 0.085 Uiso 1 1 calc R . .
H52B H -0.1953 0.2796 0.7574 0.085 Uiso 1 1 calc R . .
H52C H -0.0507 0.3091 0.7945 0.085 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0169(9) 0.0175(9) 0.0146(9) -0.0017(7) -0.0032(7) -0.0003(7)
C2 0.0131(9) 0.0202(9) 0.0161(9) -0.0024(7) -0.0020(7) -0.0014(7)
C3 0.0240(11) 0.0141(9) 0.0241(10) 0.0021(8) -0.0007(8) 0.0017(8)
C4 0.0263(11) 0.0162(10) 0.0292(11) -0.0017(8) 0.0003(9) 0.0058(8)
C5 0.0295(12) 0.0283(11) 0.0273(11) -0.0007(9) 0.0092(9) 0.0080(9)
C6 0.0326(13) 0.0363(13) 0.0282(11) 0.0033(10) 0.0152(9) 0.0079(10)
C7 0.0294(12) 0.0265(11) 0.0287(11) 0.0064(9) 0.0077(9) -0.0018(9)
C8 0.0219(10) 0.0185(10) 0.0238(10) 0.0002(8) 0.0010(8) 0.0012(8)
C9 0.0155(9) 0.0202(9) 0.0173(9) 0.0001(7) -0.0019(7) 0.0010(7)
C10 0.0215(10) 0.0207(10) 0.0225(10) -0.0004(8) 0.0011(8) 0.0028(8)
C11 0.0145(9) 0.0133(8) 0.0186(8) 0.0001(7) 0.0013(8) -0.0017(7)
C12 0.0152(9) 0.0151(8) 0.0180(8) 0.0029(7) -0.0010(8) -0.0030(7)
C13 0.0224(10) 0.0191(10) 0.0188(9) -0.0041(8) 0.0034(8) -0.0015(8)
C14 0.0223(11) 0.0159(9) 0.0275(11) -0.0017(8) 0.0017(8) 0.0023(8)
C15 0.0205(10) 0.0236(11) 0.0317(11) 0.0073(9) 0.0016(9) 0.0056(9)
C16 0.0211(11) 0.0311(11) 0.0282(11) 0.0104(9) -0.0037(9) 0.0047(9)
C17 0.0256(11) 0.0334(12) 0.0198(10) 0.0046(9) -0.0018(8) 0.0005(9)
C18 0.0210(10) 0.0221(10) 0.0190(9) 0.0007(8) 0.0014(8) 0.0010(8)
C19 0.0138(9) 0.0155(9) 0.0193(9) 0.0026(7) 0.0013(7) -0.0017(7)
C20 0.0150(9) 0.0189(9) 0.0226(10) 0.0041(8) 0.0013(8) -0.0003(7)
O1 0.0155(7) 0.0170(6) 0.0157(6) 0.0008(5) 0.0002(5) -0.0040(5)
O2 0.0186(7) 0.0149(6) 0.0163(6) 0.0018(5) -0.0028(5) -0.0019(5)
O3 0.0182(7) 0.0260(8) 0.0171(6) 0.0022(6) -0.0010(5) -0.0005(6)
O4 0.0176(7) 0.0204(7) 0.0205(7) 0.0038(6) -0.0043(5) -0.0027(6)
P 0.0143(2) 0.0171(2) 0.0138(2) 0.00204(18) -0.00127(18) -0.00243(19)
C31 0.0297(12) 0.0198(9) 0.0209(9) 0.0019(7) 0.0045(9) 0.0050(9)
C32 0.117(3) 0.0227(12) 0.0178(11) 0.0008(9) -0.0055(14) 0.0071(14)
C33 0.176(4) 0.0210(13) 0.0290(14) -0.0016(11) -0.020(2) -0.0039(19)
C34 0.137(4) 0.0240(13) 0.0341(14) 0.0101(10) -0.0109(19) -0.0022(17)
C35 0.070(2) 0.0329(13) 0.0266(12) 0.0103(10) -0.0117(13) -0.0011(13)
C36 0.0382(13) 0.0258(10) 0.0267(10) 0.0029(9) -0.0060(10) -0.0027(10)
C37 0.0218(10) 0.0182(9) 0.0149(8) 0.0002(7) 0.0015(8) 0.0013(8)
O38 0.0241(8) 0.0202(7) 0.0159(6) 0.0023(5) 0.0034(6) -0.0006(6)
C39 0.0196(10) 0.0200(9) 0.0185(9) -0.0055(8) 0.0055(8) 0.0000(8)
C40 0.0337(13) 0.0280(11) 0.0240(11) -0.0018(9) 0.0028(9) -0.0094(10)
C41 0.0416(15) 0.0339(12) 0.0335(12) -0.0076(10) 0.0114(11) -0.0195(11)
C42 0.0237(12) 0.0417(14) 0.0368(13) -0.0212(11) 0.0055(10) -0.0107(10)
C43 0.0234(11) 0.0339(12) 0.0348(12) -0.0085(10) -0.0042(10) 0.0028(9)
C44 0.0232(11) 0.0223(10) 0.0288(11) -0.0028(8) 0.0002(9) -0.0011(9)
C45 0.0191(10) 0.0170(9) 0.0160(9) -0.0008(7) 0.0031(7) 0.0000(7)
N36 0.0159(8) 0.0163(8) 0.0172(8) -0.0018(6) 0.0020(6) 0.0004(6)
O51 0.0168(7) 0.0457(9) 0.0260(8) -0.0015(7) 0.0014(6) 0.0048(7)
C51 0.0266(11) 0.0440(13) 0.0296(11) -0.0038(10) 0.0011(10) -0.0060(11)
C52 0.0383(16) 0.102(3) 0.0304(14) 0.0118(16) -0.0089(12) -0.0283(17)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.373(3) . ?
C1 C9 1.437(3) . ?
C1 C11 1.487(3) . ?
C2 O1 1.397(2) . ?
C2 C3 1.406(3) . ?
C3 C4 1.364(3) . ?
C4 C10 1.414(3) . ?
C5 C6 1.355(3) . ?
C5 C10 1.420(3) . ?
C6 C7 1.406(3) . ?
C7 C8 1.366(3) . ?
C8 C9 1.422(3) . ?
C9 C10 1.416(3) . ?
C11 C12 1.376(2) . ?
C11 C19 1.435(3) . ?
C12 O2 1.396(2) . ?
C12 C13 1.400(3) . ?
C13 C14 1.361(3) . ?
C14 C20 1.409(3) . ?
C15 C16 1.360(3) . ?
C15 C20 1.415(3) . ?
C16 C17 1.408(3) . ?
C17 C18 1.358(3) . ?
C18 C19 1.416(3) . ?
C19 C20 1.427(3) . ?
O1 P 1.6095(13) . ?
O2 P 1.6054(14) . ?
O3 P 1.4809(15) . ?
O4 P 1.4865(14) . ?
C31 C32 1.379(3) . ?
C31 C36 1.386(3) . ?
C31 C37 1.512(3) . ?
C32 C33 1.382(4) . ?
C33 C34 1.383(4) . ?
C34 C35 1.382(4) . ?
C35 C36 1.388(3) . ?
C37 O38 1.417(2) . ?
C37 C45 1.549(3) . ?
C39 C44 1.386(3) . ?
C39 C40 1.393(3) . ?
C39 C45 1.512(3) . ?
C40 C41 1.382(3) . ?
C41 C42 1.377(4) . ?
C42 C43 1.380(3) . ?
C43 C44 1.392(3) . ?
C45 N36 1.498(2) . ?
O51 C51 1.433(3) . ?
C51 C52 1.483(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C9 117.59(17) . . ?
C2 C1 C11 119.50(17) . . ?
C9 C1 C11 122.90(17) . . ?
C1 C2 O1 119.80(17) . . ?
C1 C2 C3 123.28(18) . . ?
O1 C2 C3 116.83(17) . . ?
C4 C3 C2 119.08(18) . . ?
C3 C4 C10 120.65(18) . . ?
C6 C5 C10 121.0(2) . . ?
C5 C6 C7 120.5(2) . . ?
C8 C7 C6 120.1(2) . . ?
C7 C8 C9 121.01(19) . . ?
C10 C9 C8 118.42(18) . . ?
C10 C9 C1 119.31(18) . . ?
C8 C9 C1 122.23(18) . . ?
C4 C10 C9 119.80(18) . . ?
C4 C10 C5 121.33(19) . . ?
C9 C10 C5 118.85(19) . . ?
C12 C11 C19 117.69(17) . . ?
C12 C11 C1 119.79(16) . . ?
C19 C11 C1 122.36(16) . . ?
C11 C12 O2 118.85(16) . . ?
C11 C12 C13 123.23(17) . . ?
O2 C12 C13 117.93(16) . . ?
C14 C13 C12 119.31(18) . . ?
C13 C14 C20 120.90(19) . . ?
C16 C15 C20 121.4(2) . . ?
C15 C16 C17 119.38(19) . . ?
C18 C17 C16 121.1(2) . . ?
C17 C18 C19 121.2(2) . . ?
C18 C19 C20 117.84(18) . . ?
C18 C19 C11 123.00(18) . . ?
C20 C19 C11 119.11(17) . . ?
C14 C20 C15 121.39(19) . . ?
C14 C20 C19 119.54(18) . . ?
C15 C20 C19 119.01(19) . . ?
C2 O1 P 119.23(11) . . ?
C12 O2 P 116.88(12) . . ?
O3 P O4 117.34(8) . . ?
O3 P O2 112.71(8) . . ?
O4 P O2 106.14(8) . . ?
O3 P O1 106.12(8) . . ?
O4 P O1 111.64(8) . . ?
O2 P O1 101.87(7) . . ?
C32 C31 C36 119.0(2) . . ?
C32 C31 C37 120.88(19) . . ?
C36 C31 C37 119.76(18) . . ?
C31 C32 C33 120.9(2) . . ?
C32 C33 C34 120.0(3) . . ?
C35 C34 C33 119.7(2) . . ?
C34 C35 C36 119.9(2) . . ?
C31 C36 C35 120.5(2) . . ?
O38 C37 C31 110.42(15) . . ?
O38 C37 C45 110.65(16) . . ?
C31 C37 C45 109.22(16) . . ?
C44 C39 C40 118.0(2) . . ?
C44 C39 C45 123.04(19) . . ?
C40 C39 C45 118.97(19) . . ?
C41 C40 C39 120.9(2) . . ?
C42 C41 C40 120.7(2) . . ?
C41 C42 C43 119.2(2) . . ?
C42 C43 C44 120.3(2) . . ?
C39 C44 C43 120.9(2) . . ?
N36 C45 C39 111.39(16) . . ?
N36 C45 C37 108.11(15) . . ?
C39 C45 C37 115.35(15) . . ?
O51 C51 C52 111.9(2) . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        27.92
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.051

#==END

data_imai717_2
_database_code_depnum_ccdc_archive 'CCDC 671746'
#data_im7648a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H36 N O6 P'
_chemical_formula_weight         621.64
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   8.6388(8)
_cell_length_b                   14.7982(14)
_cell_length_c                   24.537(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3136.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9410
_exptl_absorpt_correction_T_max  0.9865
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19057
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         27.91
_reflns_number_total             7133
_reflns_number_gt                6574
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+7.3573P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(17)
_refine_ls_number_reflns         7133
_refine_ls_number_parameters     409
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0758
_refine_ls_wR_factor_ref         0.1720
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_restrained_S_all      1.195
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3533(4) 0.2850(3) 0.75964(15) 0.0142(7) Uani 1 1 d . . .
C2 C 0.3327(4) 0.2064(3) 0.78853(14) 0.0126(7) Uani 1 1 d . . .
C3 C 0.4073(4) 0.1251(3) 0.77588(16) 0.0165(8) Uani 1 1 d . . .
H3 H 0.3890 0.0724 0.7970 0.020 Uiso 1 1 calc R . .
C4 C 0.5069(5) 0.1229(3) 0.73263(17) 0.0215(9) Uani 1 1 d . . .
H4 H 0.5546 0.0675 0.7226 0.026 Uiso 1 1 calc R . .
C5 C 0.6509(5) 0.2020(3) 0.65938(19) 0.0302(10) Uani 1 1 d . . .
H5 H 0.6993 0.1469 0.6491 0.036 Uiso 1 1 calc R . .
C6 C 0.6880(6) 0.2783(3) 0.6328(2) 0.0347(12) Uani 1 1 d . . .
H6 H 0.7612 0.2763 0.6040 0.042 Uiso 1 1 calc R . .
C7 C 0.6192(6) 0.3617(3) 0.6474(2) 0.0332(11) Uani 1 1 d . . .
H7 H 0.6495 0.4159 0.6296 0.040 Uiso 1 1 calc R . .
C8 C 0.5076(5) 0.3637(3) 0.68774(17) 0.0219(9) Uani 1 1 d . . .
H8 H 0.4582 0.4192 0.6965 0.026 Uiso 1 1 calc R . .
C9 C 0.4657(5) 0.2840(3) 0.71626(16) 0.0180(8) Uani 1 1 d . . .
C10 C 0.5396(5) 0.2017(3) 0.70292(16) 0.0192(8) Uani 1 1 d . . .
C11 C 0.2605(4) 0.3667(2) 0.77318(15) 0.0141(7) Uani 1 1 d . . .
C12 C 0.2532(4) 0.3954(2) 0.82663(15) 0.0140(7) Uani 1 1 d . . .
C13 C 0.1664(5) 0.4690(3) 0.84343(16) 0.0164(8) Uani 1 1 d . . .
H13 H 0.1632 0.4852 0.8809 0.020 Uiso 1 1 calc R . .
C14 C 0.0846(5) 0.5188(3) 0.80555(17) 0.0193(9) Uani 1 1 d . . .
H14 H 0.0281 0.5707 0.8167 0.023 Uiso 1 1 calc R . .
C15 C -0.0032(5) 0.5404(3) 0.71091(18) 0.0219(9) Uani 1 1 d . . .
H15 H -0.0543 0.5946 0.7213 0.026 Uiso 1 1 calc R . .
C16 C -0.0162(5) 0.5104(3) 0.65850(19) 0.0252(9) Uani 1 1 d . . .
H16 H -0.0769 0.5428 0.6328 0.030 Uiso 1 1 calc R . .
C17 C 0.0619(5) 0.4303(3) 0.64303(19) 0.0265(10) Uani 1 1 d . . .
H17 H 0.0521 0.4085 0.6068 0.032 Uiso 1 1 calc R . .
C18 C 0.1505(5) 0.3844(3) 0.67926(16) 0.0211(9) Uani 1 1 d . . .
H18 H 0.2027 0.3311 0.6678 0.025 Uiso 1 1 calc R . .
C19 C 0.1668(4) 0.4142(3) 0.73390(15) 0.0131(7) Uani 1 1 d . . .
C20 C 0.0849(4) 0.4926(3) 0.75026(16) 0.0159(8) Uani 1 1 d . . .
O1 O 0.2253(3) 0.20483(18) 0.83160(10) 0.0140(5) Uani 1 1 d . . .
O2 O 0.3388(3) 0.34947(18) 0.86656(11) 0.0138(5) Uani 1 1 d . . .
O3 O 0.1191(3) 0.26712(19) 0.91726(11) 0.0185(6) Uani 1 1 d . . .
O4 O 0.3956(3) 0.20839(19) 0.91777(11) 0.0174(6) Uani 1 1 d . . .
P P 0.26809(11) 0.25537(7) 0.88790(4) 0.0135(2) Uani 1 1 d . . .
C31 C 0.2477(5) -0.0494(3) 1.02930(17) 0.0218(8) Uani 1 1 d . . .
C32 C 0.1872(7) -0.1172(3) 0.99701(19) 0.0367(13) Uani 1 1 d . . .
H32 H 0.1532 -0.1033 0.9612 0.044 Uiso 1 1 calc R . .
C33 C 0.1753(8) -0.2043(4) 1.0156(2) 0.0464(15) Uani 1 1 d . . .
H33 H 0.1329 -0.2498 0.9928 0.056 Uiso 1 1 calc R . .
C34 C 0.2251(9) -0.2260(4) 1.0677(2) 0.0546(18) Uani 1 1 d . . .
H34 H 0.2183 -0.2864 1.0806 0.066 Uiso 1 1 calc R . .
C35 C 0.2844(10) -0.1592(4) 1.1006(3) 0.069(2) Uani 1 1 d . . .
H35 H 0.3198 -0.1732 1.1363 0.083 Uiso 1 1 calc R . .
C36 C 0.2922(8) -0.0708(4) 1.0814(2) 0.0481(17) Uani 1 1 d . . .
H36 H 0.3291 -0.0243 1.1047 0.058 Uiso 1 1 calc R . .
C37 C 0.2461(5) 0.0483(3) 1.01086(15) 0.0186(8) Uani 1 1 d . . .
H37 H 0.3395 0.0797 1.0258 0.022 Uiso 1 1 calc R . .
O38 O 0.2491(3) 0.05313(18) 0.95280(11) 0.0185(6) Uani 1 1 d . . .
H38 H 0.2776 0.1050 0.9431 0.028 Uiso 1 1 calc R . .
C39 C -0.0552(5) 0.0607(3) 1.01017(16) 0.0195(8) Uani 1 1 d . . .
C40 C -0.1243(6) -0.0131(3) 1.03458(18) 0.0249(10) Uani 1 1 d . . .
H40 H -0.0755 -0.0420 1.0646 0.030 Uiso 1 1 calc R . .
C41 C -0.2659(6) -0.0455(3) 1.0152(2) 0.0353(12) Uani 1 1 d . . .
H41 H -0.3124 -0.0965 1.0319 0.042 Uiso 1 1 calc R . .
C42 C -0.3377(6) -0.0046(3) 0.97247(19) 0.0296(10) Uani 1 1 d . . .
H42 H -0.4342 -0.0268 0.9596 0.036 Uiso 1 1 calc R . .
C43 C -0.2698(6) 0.0694(3) 0.9479(2) 0.0304(10) Uani 1 1 d . . .
H43 H -0.3201 0.0983 0.9182 0.037 Uiso 1 1 calc R . .
C44 C -0.1282(6) 0.1017(3) 0.96635(18) 0.0263(10) Uani 1 1 d . . .
H44 H -0.0812 0.1520 0.9489 0.032 Uiso 1 1 calc R . .
C45 C 0.0981(5) 0.0954(3) 1.03294(16) 0.0167(8) Uani 1 1 d . . .
H45 H 0.0956 0.0845 1.0731 0.020 Uiso 1 1 calc R . .
N36 N 0.1155(4) 0.1949(2) 1.02520(13) 0.0158(7) Uani 1 1 d . . .
H36A H 0.1236 0.2075 0.9890 0.024 Uiso 1 1 calc R . .
H36B H 0.2022 0.2143 1.0427 0.024 Uiso 1 1 calc R . .
H36C H 0.0313 0.2237 1.0391 0.024 Uiso 1 1 calc R . .
O51 O -0.1776(3) 0.2970(2) 0.89150(12) 0.0279(7) Uani 1 1 d . . .
H51 H -0.0816 0.2908 0.8955 0.042 Uiso 1 1 calc R . .
C51 C -0.2241(5) 0.2578(3) 0.84092(18) 0.0318(10) Uani 1 1 d . . .
H51A H -0.3385 0.2534 0.8402 0.038 Uiso 1 1 calc R . .
H51B H -0.1821 0.1957 0.8386 0.038 Uiso 1 1 calc R . .
C52 C -0.1723(8) 0.3092(5) 0.7929(3) 0.0510(17) Uani 1 1 d . . .
H52A H -0.1972 0.2773 0.7586 0.061 Uiso 1 1 calc R . .
H52B H -0.0598 0.3217 0.7943 0.061 Uiso 1 1 calc R . .
C53 C -0.267(2) 0.3956(14) 0.7992(6) 0.254(12) Uani 1 1 d . . .
H53A H -0.2429 0.4371 0.7693 0.381 Uiso 1 1 calc R . .
H53B H -0.2424 0.4244 0.8341 0.381 Uiso 1 1 calc R . .
H53C H -0.3779 0.3807 0.7982 0.381 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0097(17) 0.0211(19) 0.0117(17) -0.0035(14) -0.0032(13) -0.0046(15)
C2 0.0057(16) 0.0212(19) 0.0109(17) -0.0030(14) -0.0038(13) -0.0062(15)
C3 0.0148(19) 0.0157(19) 0.0188(19) 0.0014(15) -0.0016(15) -0.0022(15)
C4 0.022(2) 0.019(2) 0.024(2) -0.0029(16) -0.0058(18) 0.0095(17)
C5 0.026(2) 0.034(3) 0.031(2) 0.001(2) 0.012(2) 0.011(2)
C6 0.034(3) 0.039(3) 0.031(2) 0.012(2) 0.025(2) 0.012(2)
C7 0.034(3) 0.034(3) 0.032(3) 0.011(2) 0.015(2) -0.001(2)
C8 0.018(2) 0.020(2) 0.028(2) -0.0010(17) 0.0017(17) 0.0026(17)
C9 0.0142(19) 0.022(2) 0.0174(19) -0.0001(16) -0.0018(15) -0.0004(15)
C10 0.0150(19) 0.024(2) 0.0184(19) -0.0004(17) -0.0006(15) 0.0040(16)
C11 0.0110(17) 0.0151(17) 0.0164(17) 0.0018(14) 0.0007(15) -0.0028(15)
C12 0.0090(17) 0.0172(17) 0.0158(17) 0.0029(14) -0.0025(14) -0.0050(14)
C13 0.0159(18) 0.0182(19) 0.0150(18) -0.0033(15) 0.0003(16) 0.0003(15)
C14 0.017(2) 0.016(2) 0.025(2) -0.0008(16) 0.0077(17) 0.0014(16)
C15 0.0134(19) 0.024(2) 0.028(2) 0.0065(17) -0.0038(17) 0.0014(17)
C16 0.020(2) 0.029(2) 0.027(2) 0.0099(19) -0.0059(18) 0.0070(18)
C17 0.023(2) 0.032(2) 0.024(2) 0.0039(19) -0.0037(18) 0.0029(19)
C18 0.023(2) 0.023(2) 0.018(2) -0.0014(16) -0.0042(17) 0.0050(17)
C19 0.0062(16) 0.0171(18) 0.0160(18) 0.0040(14) 0.0016(14) -0.0028(14)
C20 0.0068(17) 0.0198(19) 0.021(2) 0.0044(16) 0.0017(14) -0.0003(15)
O1 0.0099(12) 0.0192(13) 0.0129(12) 0.0009(10) 0.0009(10) -0.0040(11)
O2 0.0093(12) 0.0142(13) 0.0179(13) 0.0000(10) -0.0027(11) -0.0031(10)
O3 0.0113(12) 0.0267(16) 0.0175(13) 0.0035(11) -0.0020(10) 0.0000(11)
O4 0.0135(13) 0.0188(14) 0.0200(14) 0.0040(11) -0.0067(11) -0.0017(11)
P 0.0109(4) 0.0163(4) 0.0135(4) 0.0015(4) -0.0010(4) -0.0018(4)
C31 0.021(2) 0.0204(19) 0.024(2) 0.0011(16) 0.0015(18) 0.0046(17)
C32 0.067(4) 0.026(2) 0.017(2) 0.0018(18) 0.001(2) 0.006(2)
C33 0.084(5) 0.027(3) 0.029(3) 0.001(2) -0.006(3) 0.000(3)
C34 0.096(5) 0.025(3) 0.043(3) 0.013(2) -0.015(3) -0.002(3)
C35 0.122(7) 0.038(3) 0.046(3) 0.019(3) -0.054(4) -0.021(4)
C36 0.075(4) 0.031(3) 0.038(3) 0.009(2) -0.036(3) -0.019(3)
C37 0.019(2) 0.0205(19) 0.0165(18) -0.0003(15) 0.0009(16) 0.0023(17)
O38 0.0204(15) 0.0178(13) 0.0172(13) 0.0022(10) -0.0003(12) -0.0001(12)
C39 0.022(2) 0.022(2) 0.0144(19) -0.0057(16) 0.0060(16) -0.0016(16)
C40 0.029(2) 0.026(2) 0.020(2) 0.0029(17) 0.0072(18) -0.0067(19)
C41 0.038(3) 0.031(2) 0.037(3) -0.008(2) 0.021(2) -0.020(2)
C42 0.022(2) 0.039(3) 0.028(2) -0.017(2) 0.0040(19) -0.008(2)
C43 0.021(2) 0.036(2) 0.034(2) -0.004(2) -0.008(2) 0.001(2)
C44 0.033(3) 0.023(2) 0.024(2) -0.0001(17) 0.0037(19) -0.0048(19)
C45 0.0185(19) 0.0171(19) 0.0145(18) 0.0003(15) 0.0005(15) 0.0004(16)
N36 0.0134(15) 0.0182(16) 0.0158(16) -0.0027(13) 0.0010(13) 0.0027(13)
O51 0.0156(14) 0.0451(19) 0.0229(15) 0.0000(15) 0.0036(12) 0.0032(14)
C51 0.018(2) 0.043(3) 0.033(2) -0.009(2) 0.0063(19) -0.008(2)
C52 0.046(4) 0.072(4) 0.034(3) 0.008(3) -0.014(3) -0.019(3)
C53 0.24(2) 0.39(3) 0.133(12) 0.053(16) -0.002(14) -0.22(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.374(5) . ?
C1 C9 1.441(5) . ?
C1 C11 1.489(5) . ?
C2 C3 1.399(6) . ?
C2 O1 1.406(4) . ?
C3 C4 1.367(6) . ?
C4 C10 1.404(6) . ?
C5 C6 1.343(7) . ?
C5 C10 1.437(6) . ?
C6 C7 1.416(7) . ?
C7 C8 1.382(6) . ?
C8 C9 1.419(6) . ?
C9 C10 1.413(6) . ?
C11 C12 1.380(5) . ?
C11 C19 1.441(5) . ?
C12 C13 1.386(5) . ?
C12 O2 1.403(4) . ?
C13 C14 1.380(6) . ?
C14 C20 1.411(6) . ?
C15 C16 1.365(6) . ?
C15 C20 1.419(6) . ?
C16 C17 1.415(6) . ?
C17 C18 1.356(6) . ?
C18 C19 1.419(5) . ?
C19 C20 1.416(5) . ?
O1 P 1.614(3) . ?
O2 P 1.608(3) . ?
O3 P 1.485(3) . ?
O4 P 1.494(3) . ?
C31 C36 1.371(6) . ?
C31 C32 1.381(7) . ?
C31 C37 1.515(5) . ?
C32 C33 1.370(7) . ?
C33 C34 1.387(7) . ?
C34 C35 1.376(8) . ?
C35 C36 1.393(7) . ?
C37 O38 1.427(4) . ?
C37 C45 1.555(5) . ?
C39 C40 1.382(6) . ?
C39 C44 1.386(6) . ?
C39 C45 1.526(6) . ?
C40 C41 1.397(7) . ?
C41 C42 1.359(7) . ?
C42 C43 1.380(7) . ?
C43 C44 1.389(7) . ?
C45 N36 1.492(5) . ?
O51 C51 1.428(5) . ?
C51 C52 1.471(8) . ?
C52 C53 1.53(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C9 117.4(4) . . ?
C2 C1 C11 120.2(3) . . ?
C9 C1 C11 122.4(3) . . ?
C1 C2 C3 123.6(3) . . ?
C1 C2 O1 119.1(3) . . ?
C3 C2 O1 117.2(3) . . ?
C4 C3 C2 118.9(4) . . ?
C3 C4 C10 120.6(4) . . ?
C6 C5 C10 121.5(4) . . ?
C5 C6 C7 120.7(4) . . ?
C8 C7 C6 119.5(4) . . ?
C7 C8 C9 120.8(4) . . ?
C10 C9 C8 119.2(4) . . ?
C10 C9 C1 119.0(4) . . ?
C8 C9 C1 121.8(4) . . ?
C4 C10 C9 120.3(4) . . ?
C4 C10 C5 121.5(4) . . ?
C9 C10 C5 118.2(4) . . ?
C12 C11 C19 117.4(3) . . ?
C12 C11 C1 119.1(3) . . ?
C19 C11 C1 123.3(3) . . ?
C11 C12 C13 123.3(3) . . ?
C11 C12 O2 119.4(3) . . ?
C13 C12 O2 117.3(3) . . ?
C14 C13 C12 119.8(4) . . ?
C13 C14 C20 120.0(4) . . ?
C16 C15 C20 121.6(4) . . ?
C15 C16 C17 119.0(4) . . ?
C18 C17 C16 120.9(4) . . ?
C17 C18 C19 121.3(4) . . ?
C20 C19 C18 118.2(3) . . ?
C20 C19 C11 119.4(3) . . ?
C18 C19 C11 122.4(4) . . ?
C14 C20 C19 119.9(4) . . ?
C14 C20 C15 121.1(4) . . ?
C19 C20 C15 118.9(4) . . ?
C2 O1 P 119.0(2) . . ?
C12 O2 P 116.5(2) . . ?
O3 P O4 117.07(16) . . ?
O3 P O2 112.68(16) . . ?
O4 P O2 106.44(15) . . ?
O3 P O1 105.73(15) . . ?
O4 P O1 111.89(16) . . ?
O2 P O1 102.09(14) . . ?
C36 C31 C32 118.2(4) . . ?
C36 C31 C37 120.0(4) . . ?
C32 C31 C37 121.2(4) . . ?
C33 C32 C31 121.4(5) . . ?
C32 C33 C34 120.1(5) . . ?
C35 C34 C33 119.4(5) . . ?
C34 C35 C36 119.6(5) . . ?
C31 C36 C35 121.3(5) . . ?
O38 C37 C31 110.3(3) . . ?
O38 C37 C45 109.9(3) . . ?
C31 C37 C45 109.4(3) . . ?
C40 C39 C44 119.0(4) . . ?
C40 C39 C45 118.9(4) . . ?
C44 C39 C45 122.1(4) . . ?
C39 C40 C41 120.1(4) . . ?
C42 C41 C40 120.7(4) . . ?
C41 C42 C43 119.7(4) . . ?
C42 C43 C44 120.3(4) . . ?
C39 C44 C43 120.2(4) . . ?
N36 C45 C39 111.9(3) . . ?
N36 C45 C37 108.4(3) . . ?
C39 C45 C37 115.8(3) . . ?
O51 C51 C52 113.5(4) . . ?
C51 C52 C53 100.9(7) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        27.91
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.086

#==END

data_imai717_3
_database_code_depnum_ccdc_archive 'CCDC 671747'
#data_im7683a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H36 N O6 P'
_chemical_formula_weight         621.64
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   8.7098(6)
_cell_length_b                   14.6885(11)
_cell_length_c                   24.5732(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3143.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    6002
_cell_measurement_theta_min      1.62
_cell_measurement_theta_max      27.87

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9287
_exptl_absorpt_correction_T_max  0.9932
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      130(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  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19638
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         27.87
_reflns_number_total             7197
_reflns_number_gt                6002
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.1006P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.22(10)
_refine_ls_number_reflns         7197
_refine_ls_number_parameters     411
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0542
_refine_ls_wR_factor_ref         0.1091
_refine_ls_wR_factor_gt          0.1031
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3473(3) 0.27832(16) 0.76035(9) 0.0131(5) Uani 1 1 d . . .
C2 C 0.3331(3) 0.20150(17) 0.79107(9) 0.0147(5) Uani 1 1 d . . .
C3 C 0.4056(3) 0.11875(17) 0.77783(10) 0.0190(6) Uani 1 1 d . . .
H3 H 0.3914 0.0665 0.8000 0.023 Uiso 1 1 calc R . .
C4 C 0.4961(3) 0.11470(17) 0.73291(10) 0.0207(6) Uani 1 1 d . . .
H4 H 0.5412 0.0584 0.7227 0.025 Uiso 1 1 calc R . .
C5 C 0.6256(3) 0.19141(19) 0.65597(10) 0.0256(6) Uani 1 1 d . . .
H5 H 0.6725 0.1356 0.6456 0.031 Uiso 1 1 calc R . .
C6 C 0.6568(3) 0.2681(2) 0.62730(11) 0.0299(7) Uani 1 1 d . . .
H6 H 0.7239 0.2652 0.5969 0.036 Uiso 1 1 calc R . .
C7 C 0.5910(3) 0.3516(2) 0.64215(10) 0.0251(6) Uani 1 1 d . . .
H7 H 0.6165 0.4053 0.6226 0.030 Uiso 1 1 calc R . .
C8 C 0.4900(3) 0.35582(18) 0.68483(9) 0.0185(6) Uani 1 1 d . . .
H8 H 0.4447 0.4125 0.6942 0.022 Uiso 1 1 calc R . .
C9 C 0.4522(3) 0.27659(17) 0.71522(9) 0.0151(5) Uani 1 1 d . . .
C10 C 0.5239(3) 0.19300(18) 0.70119(10) 0.0183(6) Uani 1 1 d . . .
C11 C 0.2576(3) 0.36119(16) 0.77461(9) 0.0134(5) Uani 1 1 d . . .
C12 C 0.2590(3) 0.39407(16) 0.82707(9) 0.0144(5) Uani 1 1 d . . .
C13 C 0.1763(3) 0.47032(16) 0.84334(9) 0.0148(5) Uani 1 1 d . . .
H13 H 0.1803 0.4903 0.8801 0.018 Uiso 1 1 calc R . .
C14 C 0.0897(3) 0.51598(17) 0.80643(10) 0.0168(5) Uani 1 1 d . . .
H14 H 0.0372 0.5698 0.8171 0.020 Uiso 1 1 calc R . .
C15 C -0.0214(3) 0.52791(18) 0.71407(10) 0.0216(6) Uani 1 1 d . . .
H15 H -0.0745 0.5818 0.7243 0.026 Uiso 1 1 calc R . .
C16 C -0.0405(3) 0.49374(19) 0.66336(10) 0.0264(7) Uani 1 1 d . . .
H16 H -0.1056 0.5238 0.6381 0.032 Uiso 1 1 calc R . .
C17 C 0.0362(3) 0.41372(19) 0.64829(10) 0.0267(7) Uani 1 1 d . . .
H17 H 0.0217 0.3897 0.6128 0.032 Uiso 1 1 calc R . .
C18 C 0.1305(3) 0.37017(18) 0.68334(10) 0.0197(6) Uani 1 1 d . . .
H18 H 0.1798 0.3155 0.6724 0.024 Uiso 1 1 calc R . .
C19 C 0.1569(3) 0.40520(16) 0.73644(9) 0.0149(5) Uani 1 1 d . . .
C20 C 0.0766(3) 0.48459(17) 0.75224(9) 0.0165(5) Uani 1 1 d . . .
O1 O 0.2348(2) 0.20131(11) 0.83603(6) 0.0151(4) Uani 1 1 d . . .
O2 O 0.3484(2) 0.34937(11) 0.86608(6) 0.0144(4) Uani 1 1 d . . .
O3 O 0.13958(19) 0.26918(11) 0.92177(6) 0.0182(4) Uani 1 1 d . . .
O4 O 0.4137(2) 0.21073(11) 0.91821(6) 0.0171(4) Uani 1 1 d . . .
P P 0.28312(7) 0.25563(4) 0.89033(2) 0.01351(14) Uani 1 1 d . . .
C31 C 0.2635(3) -0.05495(16) 1.02377(9) 0.0166(5) Uani 1 1 d . . .
C32 C 0.1838(3) -0.12106(18) 0.99556(10) 0.0260(7) Uani 1 1 d . . .
H32 H 0.1337 -0.1055 0.9625 0.031 Uiso 1 1 calc R . .
C33 C 0.1756(4) -0.20923(18) 1.01454(11) 0.0299(7) Uani 1 1 d . . .
H33 H 0.1186 -0.2535 0.9949 0.036 Uiso 1 1 calc R . .
C34 C 0.2498(4) -0.23335(18) 1.06197(11) 0.0302(7) Uani 1 1 d . . .
H34 H 0.2436 -0.2939 1.0753 0.036 Uiso 1 1 calc R . .
C35 C 0.3329(4) -0.1687(2) 1.08971(12) 0.0391(8) Uani 1 1 d . . .
H35 H 0.3868 -0.1851 1.1218 0.047 Uiso 1 1 calc R . .
C36 C 0.3383(3) -0.07982(19) 1.07112(11) 0.0271(7) Uani 1 1 d . . .
H36 H 0.3940 -0.0354 1.0911 0.033 Uiso 1 1 calc R . .
C37 C 0.2607(3) 0.04359(16) 1.00688(9) 0.0170(5) Uani 1 1 d . . .
H37 H 0.3547 0.0741 1.0215 0.020 Uiso 1 1 calc R . .
O38 O 0.2624(2) 0.05051(12) 0.94921(6) 0.0200(4) Uani 1 1 d . . .
H38 H 0.3223 0.0924 0.9398 0.030 Uiso 1 1 calc R . .
C39 C -0.0353(3) 0.06097(17) 1.00777(10) 0.0180(6) Uani 1 1 d . . .
C40 C -0.1128(3) -0.00973(18) 1.03328(10) 0.0226(6) Uani 1 1 d . . .
H40 H -0.0694 -0.0376 1.0646 0.027 Uiso 1 1 calc R . .
C41 C -0.2518(4) -0.03996(19) 1.01367(11) 0.0308(7) Uani 1 1 d . . .
H41 H -0.3027 -0.0891 1.0311 0.037 Uiso 1 1 calc R . .
C42 C -0.3173(3) 0.0008(2) 0.96888(11) 0.0313(7) Uani 1 1 d . . .
H42 H -0.4140 -0.0195 0.9557 0.038 Uiso 1 1 calc R . .
C43 C -0.2413(3) 0.0714(2) 0.94312(12) 0.0304(7) Uani 1 1 d . . .
H43 H -0.2859 0.0995 0.9121 0.037 Uiso 1 1 calc R . .
C44 C -0.1006(3) 0.10114(18) 0.96224(11) 0.0228(6) Uani 1 1 d . . .
H44 H -0.0485 0.1492 0.9441 0.027 Uiso 1 1 calc R . .
C45 C 0.1179(3) 0.09106(16) 1.03117(10) 0.0167(5) Uani 1 1 d . . .
H45 H 0.1158 0.0752 1.0707 0.020 Uiso 1 1 calc R . .
N36 N 0.1393(2) 0.19170(13) 1.02789(8) 0.0162(5) Uani 1 1 d . . .
H36A H 0.1502 0.2085 0.9925 0.024 Uiso 1 1 calc R . .
H36B H 0.2248 0.2079 1.0468 0.024 Uiso 1 1 calc R . .
H36C H 0.0559 0.2201 1.0424 0.024 Uiso 1 1 calc R . .
O51 O -0.1414(2) 0.32781(13) 0.88995(7) 0.0229(4) Uani 1 1 d . . .
H51 H -0.0517 0.3126 0.8986 0.034 Uiso 1 1 calc R . .
C51 C -0.1590(3) 0.32195(19) 0.83158(10) 0.0214(6) Uani 1 1 d . . .
H51B H -0.0579 0.3352 0.8140 0.026 Uiso 1 1 calc R . .
C52 C -0.2743(3) 0.3933(2) 0.81392(10) 0.0282(7) Uani 1 1 d . . .
H52A H -0.3739 0.3805 0.8308 0.042 Uiso 1 1 calc R . .
H52B H -0.2851 0.3918 0.7742 0.042 Uiso 1 1 calc R . .
H52C H -0.2386 0.4536 0.8253 0.042 Uiso 1 1 calc R . .
C53 C -0.2090(4) 0.2272(2) 0.81605(13) 0.0418(8) Uani 1 1 d . . .
H53A H -0.1342 0.1830 0.8298 0.063 Uiso 1 1 calc R . .
H53B H -0.2152 0.2225 0.7763 0.063 Uiso 1 1 calc R . .
H53C H -0.3099 0.2146 0.8319 0.063 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0127(12) 0.0151(12) 0.0115(11) -0.0037(9) -0.0046(9) -0.0010(10)
C2 0.0095(12) 0.0202(13) 0.0145(12) -0.0027(10) -0.0017(10) -0.0034(10)
C3 0.0222(15) 0.0126(13) 0.0222(13) 0.0023(10) -0.0043(11) -0.0010(11)
C4 0.0220(15) 0.0167(13) 0.0233(13) -0.0031(11) -0.0026(12) 0.0058(11)
C5 0.0263(17) 0.0255(15) 0.0252(14) -0.0039(12) 0.0055(12) 0.0089(12)
C6 0.0283(16) 0.0383(18) 0.0230(14) -0.0005(13) 0.0106(12) 0.0072(14)
C7 0.0245(16) 0.0293(16) 0.0214(14) 0.0042(12) 0.0054(12) -0.0006(12)
C8 0.0180(14) 0.0214(14) 0.0160(12) 0.0003(11) -0.0012(11) 0.0022(11)
C9 0.0132(13) 0.0189(13) 0.0131(12) -0.0013(10) -0.0027(9) -0.0011(10)
C10 0.0165(14) 0.0237(14) 0.0148(12) -0.0018(10) -0.0013(11) 0.0032(11)
C11 0.0098(13) 0.0155(12) 0.0148(11) 0.0032(9) 0.0023(10) -0.0036(9)
C12 0.0127(13) 0.0162(12) 0.0142(11) 0.0058(9) -0.0022(10) -0.0040(10)
C13 0.0168(14) 0.0144(12) 0.0132(12) -0.0026(10) 0.0034(10) -0.0038(10)
C14 0.0160(13) 0.0126(12) 0.0218(13) -0.0014(10) 0.0046(11) 0.0008(10)
C15 0.0162(14) 0.0206(14) 0.0281(15) 0.0055(11) 0.0033(11) 0.0057(11)
C16 0.0249(16) 0.0334(17) 0.0208(14) 0.0075(12) -0.0045(12) 0.0064(13)
C17 0.0264(16) 0.0363(17) 0.0174(13) 0.0005(12) -0.0033(12) 0.0055(13)
C18 0.0206(15) 0.0215(14) 0.0171(13) -0.0019(11) -0.0027(11) 0.0049(12)
C19 0.0123(12) 0.0157(12) 0.0168(12) 0.0037(10) 0.0011(10) -0.0017(10)
C20 0.0130(13) 0.0168(13) 0.0196(13) 0.0030(11) 0.0018(10) -0.0021(10)
O1 0.0152(10) 0.0168(9) 0.0132(8) 0.0010(7) 0.0009(7) -0.0045(7)
O2 0.0154(9) 0.0160(9) 0.0119(8) 0.0016(7) -0.0025(7) -0.0009(7)
O3 0.0141(9) 0.0240(10) 0.0165(8) 0.0026(7) -0.0012(7) 0.0004(8)
O4 0.0145(9) 0.0189(9) 0.0179(8) 0.0027(7) -0.0020(7) -0.0022(7)
P 0.0122(3) 0.0161(3) 0.0122(3) 0.0021(3) -0.0014(2) -0.0020(3)
C31 0.0182(14) 0.0184(12) 0.0132(11) -0.0026(10) 0.0036(10) 0.0057(10)
C32 0.0417(19) 0.0192(14) 0.0170(13) 0.0006(11) -0.0079(13) 0.0042(13)
C33 0.044(2) 0.0209(15) 0.0246(14) -0.0027(12) -0.0073(14) -0.0016(13)
C34 0.044(2) 0.0188(14) 0.0278(14) 0.0073(11) -0.0037(13) -0.0018(13)
C35 0.054(2) 0.0332(17) 0.0299(16) 0.0131(14) -0.0183(16) -0.0053(16)
C36 0.0309(17) 0.0250(15) 0.0255(14) 0.0046(12) -0.0098(13) -0.0053(13)
C37 0.0172(14) 0.0182(12) 0.0156(12) 0.0010(10) 0.0011(11) 0.0003(10)
O38 0.0221(11) 0.0215(10) 0.0165(8) 0.0031(7) 0.0019(8) -0.0021(8)
C39 0.0190(14) 0.0182(13) 0.0168(12) -0.0052(10) 0.0042(11) 0.0022(11)
C40 0.0282(16) 0.0212(14) 0.0184(13) -0.0036(11) 0.0049(12) -0.0042(12)
C41 0.0321(18) 0.0288(15) 0.0314(15) -0.0068(13) 0.0121(14) -0.0145(13)
C42 0.0202(16) 0.0387(18) 0.0352(16) -0.0178(14) 0.0048(13) -0.0087(13)
C43 0.0263(17) 0.0351(17) 0.0298(15) -0.0011(13) -0.0064(13) 0.0017(13)
C44 0.0192(14) 0.0245(15) 0.0248(14) -0.0001(12) 0.0010(12) -0.0002(12)
C45 0.0168(13) 0.0164(13) 0.0170(12) 0.0004(10) 0.0022(11) 0.0001(10)
N36 0.0134(11) 0.0183(11) 0.0169(10) 0.0005(9) 0.0014(9) 0.0027(9)
O51 0.0160(10) 0.0353(11) 0.0174(9) 0.0012(9) 0.0000(8) 0.0057(9)
C51 0.0157(14) 0.0337(16) 0.0149(12) 0.0026(11) 0.0031(11) -0.0019(12)
C52 0.0252(16) 0.0355(16) 0.0239(14) 0.0064(12) -0.0020(13) -0.0034(14)
C53 0.043(2) 0.0371(18) 0.0451(18) -0.0128(15) -0.0105(16) 0.0008(16)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.363(3) . ?
C1 C9 1.437(3) . ?
C1 C11 1.488(3) . ?
C2 O1 1.398(3) . ?
C2 C3 1.408(3) . ?
C3 C4 1.357(4) . ?
C4 C10 1.411(3) . ?
C5 C6 1.356(4) . ?
C5 C10 1.421(3) . ?
C6 C7 1.402(4) . ?
C7 C8 1.370(3) . ?
C8 C9 1.421(3) . ?
C9 C10 1.420(3) . ?
C11 C12 1.377(3) . ?
C11 C19 1.438(3) . ?
C12 C13 1.390(3) . ?
C12 O2 1.399(3) . ?
C13 C14 1.357(3) . ?
C14 C20 1.414(3) . ?
C15 C16 1.354(4) . ?
C15 C20 1.419(3) . ?
C16 C17 1.402(4) . ?
C17 C18 1.351(4) . ?
C18 C19 1.421(3) . ?
C19 C20 1.414(3) . ?
O1 P 1.6107(16) . ?
O2 P 1.6046(17) . ?
O3 P 1.4830(18) . ?
O4 P 1.4823(18) . ?
C31 C32 1.381(4) . ?
C31 C36 1.383(3) . ?
C31 C37 1.506(3) . ?
C32 C33 1.378(4) . ?
C33 C34 1.379(4) . ?
C34 C35 1.375(4) . ?
C35 C36 1.383(4) . ?
C37 O38 1.421(3) . ?
C37 C45 1.546(3) . ?
C39 C44 1.387(4) . ?
C39 C40 1.388(4) . ?
C39 C45 1.518(4) . ?
C40 C41 1.377(4) . ?
C41 C42 1.376(4) . ?
C42 C43 1.384(4) . ?
C43 C44 1.383(4) . ?
C45 N36 1.492(3) . ?
O51 C51 1.445(3) . ?
C51 C53 1.507(4) . ?
C51 C52 1.515(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C9 118.1(2) . . ?
C2 C1 C11 119.9(2) . . ?
C9 C1 C11 122.0(2) . . ?
C1 C2 O1 119.7(2) . . ?
C1 C2 C3 123.1(2) . . ?
O1 C2 C3 117.1(2) . . ?
C4 C3 C2 119.1(2) . . ?
C3 C4 C10 120.9(2) . . ?
C6 C5 C10 121.2(2) . . ?
C5 C6 C7 120.6(2) . . ?
C8 C7 C6 120.1(3) . . ?
C7 C8 C9 120.9(2) . . ?
C10 C9 C8 118.6(2) . . ?
C10 C9 C1 118.8(2) . . ?
C8 C9 C1 122.6(2) . . ?
C4 C10 C9 119.7(2) . . ?
C4 C10 C5 121.7(2) . . ?
C9 C10 C5 118.6(2) . . ?
C12 C11 C19 117.3(2) . . ?
C12 C11 C1 120.2(2) . . ?
C19 C11 C1 122.3(2) . . ?
C11 C12 C13 123.2(2) . . ?
C11 C12 O2 118.8(2) . . ?
C13 C12 O2 118.0(2) . . ?
C14 C13 C12 119.6(2) . . ?
C13 C14 C20 120.9(2) . . ?
C16 C15 C20 121.1(3) . . ?
C15 C16 C17 119.7(2) . . ?
C18 C17 C16 121.2(2) . . ?
C17 C18 C19 120.8(2) . . ?
C20 C19 C18 118.1(2) . . ?
C20 C19 C11 119.6(2) . . ?
C18 C19 C11 122.3(2) . . ?
C14 C20 C19 119.2(2) . . ?
C14 C20 C15 121.7(2) . . ?
C19 C20 C15 119.1(2) . . ?
C2 O1 P 119.58(14) . . ?
C12 O2 P 117.38(15) . . ?
O4 P O3 117.76(10) . . ?
O4 P O2 106.35(10) . . ?
O3 P O2 112.15(9) . . ?
O4 P O1 111.28(10) . . ?
O3 P O1 106.12(9) . . ?
O2 P O1 102.12(8) . . ?
C32 C31 C36 118.3(2) . . ?
C32 C31 C37 122.0(2) . . ?
C36 C31 C37 119.6(2) . . ?
C33 C32 C31 121.1(2) . . ?
C32 C33 C34 120.2(3) . . ?
C35 C34 C33 119.2(3) . . ?
C34 C35 C36 120.4(3) . . ?
C31 C36 C35 120.7(3) . . ?
O38 C37 C31 110.09(19) . . ?
O38 C37 C45 111.2(2) . . ?
C31 C37 C45 109.9(2) . . ?
C44 C39 C40 118.9(3) . . ?
C44 C39 C45 122.8(2) . . ?
C40 C39 C45 118.3(2) . . ?
C41 C40 C39 120.7(3) . . ?
C42 C41 C40 120.3(3) . . ?
C41 C42 C43 119.6(3) . . ?
C44 C43 C42 120.4(3) . . ?
C43 C44 C39 120.2(3) . . ?
N36 C45 C39 112.2(2) . . ?
N36 C45 C37 108.99(19) . . ?
C39 C45 C37 115.4(2) . . ?
O51 C51 C53 109.7(2) . . ?
O51 C51 C52 108.3(2) . . ?
C53 C51 C52 112.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        27.87
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.056

#==END