# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Pradyut Ghosh'
_publ_contact_author_address     
;
Department of Inorganic Chemistry
Indian Association for the Cultivation of Science
2A & 2B Raja S. C. Mullick Road
Jadavpur
Kolkata
West Bengal
700032
INDIA
;

_publ_contact_author_email       ICPG@IACS.RES.IN

_publ_section_title              
;
Trapped Inorganic Phosphate Dimer
;
loop_
_publ_author_name
'Pradyut Ghosh'
'P. S. Lakshminarayanan'
'I. Ravikumar'
'E. Suresh'

# Attachment '95ps2m.cif'

data_95ps2m
_database_code_depnum_ccdc_archive 'CCDC 655559'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H18 F15 N7 O3'
_chemical_formula_weight         773.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           TRICLINIC
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.2984(10)
_cell_length_b                   13.3540(14)
_cell_length_c                   13.7161(14)
_cell_angle_alpha                118.317(2)
_cell_angle_beta                 90.295(2)
_cell_angle_gamma                96.329(2)
_cell_volume                     1487.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCKS
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8927
_exptl_absorpt_correction_T_max  0.9600
_exptl_absorpt_process_details   BRUKER-SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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 SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12837
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         28.29
_reflns_number_total             6733
_reflns_number_gt                5311
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SMART'
_computing_cell_refinement       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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 w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.9554P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6733
_refine_ls_number_parameters     493
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1297
_refine_ls_wR_factor_gt          0.1215
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.01665(16) 0.71251(12) 0.33186(12) 0.0240(3) Uani 1 d . . .
F2 F 0.03384(17) 0.66354(13) 0.49951(12) 0.0285(4) Uani 1 d . . .
F3 F 0.24190(18) 0.53884(14) 0.50819(13) 0.0336(4) Uani 1 d . . .
F4 F 0.42907(17) 0.46165(14) 0.34472(14) 0.0331(4) Uani 1 d . . .
F5 F 0.41311(16) 0.51086(13) 0.17642(13) 0.0267(4) Uani 1 d . . .
F6 F -0.45149(16) 0.70091(11) 0.13775(12) 0.0228(3) Uani 1 d . . .
F7 F -0.58178(15) 0.83822(12) 0.32093(12) 0.0232(3) Uani 1 d . . .
F8 F -0.47613(16) 1.06488(12) 0.44107(12) 0.0251(3) Uani 1 d . . .
F9 F -0.23804(17) 1.14965(12) 0.37926(12) 0.0275(4) Uani 1 d . . .
F10 F -0.10279(15) 1.01358(12) 0.20125(12) 0.0240(3) Uani 1 d . . .
F11 F 0.09904(16) 0.87100(12) 0.24998(12) 0.0242(3) Uani 1 d . . .
F12 F 0.12209(17) 0.95072(14) 0.46973(13) 0.0310(4) Uani 1 d . . .
F13 F 0.22269(19) 1.17389(15) 0.60796(13) 0.0378(4) Uani 1 d . . .
F14 F 0.33003(19) 1.31149(13) 0.52248(14) 0.0380(4) Uani 1 d . . .
F15 F 0.33799(16) 1.22492(12) 0.30072(13) 0.0277(4) Uani 1 d . . .
O1 O 0.15364(18) 0.45205(13) 0.02848(14) 0.0181(4) Uani 1 d . . .
O2 O -0.20185(19) 0.88639(14) -0.02035(15) 0.0223(4) Uani 1 d . . .
O3 O 0.32185(18) 0.84010(14) 0.10916(14) 0.0182(4) Uani 1 d . . .
N1 N 0.1999(2) 0.66961(16) -0.18297(16) 0.0153(4) Uani 1 d . . .
N2 N 0.2186(2) 0.58805(18) -0.02296(17) 0.0170(4) Uani 1 d . . .
N3 N 0.2048(2) 0.63880(17) 0.16091(17) 0.0169(4) Uani 1 d . . .
N4 N -0.0876(2) 0.72738(18) -0.08836(18) 0.0211(5) Uani 1 d . . .
N5 N -0.2070(2) 0.77877(18) 0.06922(18) 0.0189(4) Uani 1 d . . .
N6 N 0.3233(2) 0.91230(18) -0.01194(17) 0.0191(4) Uani 1 d . . .
N7 N 0.2223(2) 1.00510(17) 0.15340(17) 0.0178(4) Uani 1 d . . .
C1 C 0.2616(3) 0.5644(2) -0.2059(2) 0.0182(5) Uani 1 d . . .
H1A H 0.3653 0.5827 -0.1872 0.022 Uiso 1 calc R . .
H1B H 0.2465 0.5105 -0.2846 0.022 Uiso 1 calc R . .
C2 C 0.1940(3) 0.5089(2) -0.1408(2) 0.0188(5) Uani 1 d . . .
H2A H 0.0907 0.4881 -0.1606 0.023 Uiso 1 calc R . .
H2B H 0.2364 0.4395 -0.1586 0.023 Uiso 1 calc R . .
C3 C 0.1911(2) 0.55346(19) 0.0522(2) 0.0150(5) Uani 1 d . . .
C4 C 0.2153(3) 0.61434(19) 0.2494(2) 0.0173(5) Uani 1 d . . .
C5 C 0.1216(3) 0.6530(2) 0.3344(2) 0.0181(5) Uani 1 d . . .
C6 C 0.1310(3) 0.6287(2) 0.4215(2) 0.0205(5) Uani 1 d . . .
C7 C 0.2341(3) 0.5645(2) 0.4251(2) 0.0238(6) Uani 1 d . . .
C8 C 0.3281(3) 0.5241(2) 0.3419(2) 0.0227(6) Uani 1 d . . .
C9 C 0.3190(3) 0.5497(2) 0.2553(2) 0.0200(5) Uani 1 d . . .
C10 C 0.0611(3) 0.6452(2) -0.24536(19) 0.0176(5) Uani 1 d . . .
H10A H 0.0132 0.5711 -0.2588 0.021 Uiso 1 calc R . .
H10B H 0.0786 0.6411 -0.3168 0.021 Uiso 1 calc R . .
C11 C -0.0382(3) 0.7353(2) -0.1850(2) 0.0201(5) Uani 1 d . . .
H11A H 0.0134 0.8110 -0.1620 0.024 Uiso 1 calc R . .
H11B H -0.1208 0.7238 -0.2343 0.024 Uiso 1 calc R . .
C12 C -0.1669(3) 0.8025(2) -0.0148(2) 0.0176(5) Uani 1 d . . .
C13 C -0.2767(3) 0.8531(2) 0.1606(2) 0.0161(5) Uani 1 d . . .
C14 C -0.3986(3) 0.81236(19) 0.19560(19) 0.0160(5) Uani 1 d . . .
C15 C -0.4656(3) 0.8815(2) 0.2888(2) 0.0174(5) Uani 1 d . . .
C16 C -0.4135(3) 0.9958(2) 0.34963(19) 0.0177(5) Uani 1 d . . .
C17 C -0.2924(3) 1.0394(2) 0.3176(2) 0.0189(5) Uani 1 d . . .
C18 C -0.2250(3) 0.9685(2) 0.2252(2) 0.0177(5) Uani 1 d . . .
C19 C 0.3038(3) 0.7494(2) -0.20081(19) 0.0171(5) Uani 1 d . . .
H19A H 0.2514 0.7955 -0.2223 0.021 Uiso 1 calc R . .
H19B H 0.3629 0.7061 -0.2611 0.021 Uiso 1 calc R . .
C20 C 0.4010(3) 0.8273(2) -0.0977(2) 0.0187(5) Uani 1 d . . .
H20A H 0.4407 0.7815 -0.0690 0.022 Uiso 1 calc R . .
H20B H 0.4812 0.8662 -0.1168 0.022 Uiso 1 calc R . .
C21 C 0.2917(2) 0.91214(19) 0.08303(19) 0.0152(5) Uani 1 d . . .
C22 C 0.2219(3) 1.0445(2) 0.2674(2) 0.0171(5) Uani 1 d . . .
C23 C 0.1645(3) 0.9781(2) 0.3146(2) 0.0192(5) Uani 1 d . . .
C24 C 0.1691(3) 1.0200(2) 0.4275(2) 0.0243(6) Uani 1 d . . .
C25 C 0.2210(3) 1.1333(2) 0.4982(2) 0.0265(6) Uani 1 d . . .
C26 C 0.2745(3) 1.2023(2) 0.4543(2) 0.0256(6) Uani 1 d . . .
C27 C 0.2777(3) 1.1572(2) 0.3412(2) 0.0223(6) Uani 1 d . . .
H6C H 0.305(3) 0.967(2) -0.024(2) 0.018(7) Uiso 1 d . . .
H7C H 0.212(3) 1.051(2) 0.132(2) 0.020(7) Uiso 1 d . . .
H3C H 0.225(3) 0.710(2) 0.178(2) 0.015(7) Uiso 1 d . . .
H5C H -0.202(3) 0.711(3) 0.060(2) 0.031(8) Uiso 1 d . . .
H2C H 0.242(3) 0.660(3) 0.001(2) 0.026(8) Uiso 1 d . . .
H4C H -0.069(3) 0.671(3) -0.081(3) 0.036(9) Uiso 1 d . . .

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
F1 0.0266(8) 0.0197(8) 0.0266(8) 0.0106(6) 0.0062(6) 0.0085(6)
F2 0.0324(9) 0.0294(9) 0.0199(8) 0.0092(7) 0.0081(7) 0.0012(7)
F3 0.0434(10) 0.0414(10) 0.0245(8) 0.0231(8) 0.0010(7) 0.0028(8)
F4 0.0317(9) 0.0422(10) 0.0414(10) 0.0312(8) 0.0030(7) 0.0129(8)
F5 0.0250(8) 0.0325(9) 0.0326(9) 0.0221(7) 0.0114(7) 0.0119(7)
F6 0.0269(8) 0.0139(7) 0.0240(8) 0.0073(6) 0.0024(6) -0.0034(6)
F7 0.0198(7) 0.0271(8) 0.0221(8) 0.0122(7) 0.0052(6) -0.0020(6)
F8 0.0322(9) 0.0232(8) 0.0192(8) 0.0084(6) 0.0065(6) 0.0097(7)
F9 0.0403(9) 0.0116(7) 0.0245(8) 0.0056(6) -0.0036(7) -0.0050(6)
F10 0.0212(8) 0.0198(8) 0.0330(9) 0.0155(7) 0.0037(6) -0.0036(6)
F11 0.0278(8) 0.0172(7) 0.0301(8) 0.0137(7) 0.0031(7) 0.0003(6)
F12 0.0378(9) 0.0395(10) 0.0317(9) 0.0275(8) 0.0133(7) 0.0164(8)
F13 0.0490(11) 0.0462(10) 0.0191(8) 0.0118(8) 0.0022(7) 0.0281(9)
F14 0.0495(11) 0.0186(8) 0.0309(9) -0.0005(7) -0.0108(8) 0.0066(7)
F15 0.0321(9) 0.0159(7) 0.0362(9) 0.0140(7) -0.0008(7) -0.0010(6)
O1 0.0248(9) 0.0100(8) 0.0203(9) 0.0085(7) 0.0032(7) -0.0001(7)
O2 0.0307(10) 0.0169(9) 0.0271(10) 0.0154(8) 0.0082(8) 0.0104(8)
O3 0.0219(9) 0.0138(8) 0.0202(9) 0.0089(7) -0.0010(7) 0.0030(7)
N1 0.0172(10) 0.0124(10) 0.0182(10) 0.0089(8) 0.0016(8) 0.0017(8)
N2 0.0233(11) 0.0094(10) 0.0182(11) 0.0071(8) 0.0000(8) -0.0013(8)
N3 0.0249(11) 0.0093(10) 0.0179(11) 0.0081(8) -0.0005(8) -0.0005(8)
N4 0.0279(12) 0.0172(11) 0.0270(12) 0.0157(10) 0.0120(9) 0.0117(9)
N5 0.0252(11) 0.0117(10) 0.0260(12) 0.0130(9) 0.0098(9) 0.0077(9)
N6 0.0270(12) 0.0138(10) 0.0198(11) 0.0102(9) 0.0048(9) 0.0043(9)
N7 0.0257(11) 0.0133(10) 0.0191(11) 0.0109(9) 0.0012(9) 0.0053(9)
C1 0.0228(13) 0.0127(11) 0.0197(12) 0.0078(10) 0.0031(10) 0.0035(10)
C2 0.0233(13) 0.0134(11) 0.0202(13) 0.0081(10) 0.0023(10) 0.0032(10)
C3 0.0131(11) 0.0130(11) 0.0202(12) 0.0088(10) 0.0004(9) 0.0022(9)
C4 0.0214(12) 0.0117(11) 0.0196(13) 0.0088(10) 0.0002(10) -0.0014(10)
C5 0.0198(12) 0.0125(11) 0.0194(13) 0.0060(10) -0.0017(10) -0.0002(10)
C6 0.0231(13) 0.0161(12) 0.0154(12) 0.0032(10) 0.0029(10) -0.0041(10)
C7 0.0317(14) 0.0229(13) 0.0178(13) 0.0125(11) -0.0037(11) -0.0054(11)
C8 0.0227(13) 0.0214(13) 0.0276(14) 0.0148(12) -0.0021(11) 0.0019(11)
C9 0.0198(12) 0.0190(12) 0.0216(13) 0.0103(11) 0.0030(10) 0.0017(10)
C10 0.0207(12) 0.0168(12) 0.0148(12) 0.0073(10) -0.0001(10) 0.0011(10)
C11 0.0226(13) 0.0214(13) 0.0231(13) 0.0158(11) 0.0038(10) 0.0043(10)
C12 0.0163(12) 0.0161(12) 0.0228(13) 0.0116(10) 0.0034(10) 0.0006(10)
C13 0.0170(12) 0.0160(12) 0.0196(12) 0.0114(10) 0.0011(10) 0.0048(9)
C14 0.0195(12) 0.0120(11) 0.0177(12) 0.0090(10) -0.0032(10) -0.0022(9)
C15 0.0161(12) 0.0200(13) 0.0204(13) 0.0135(11) 0.0002(10) 0.0008(10)
C16 0.0212(12) 0.0190(12) 0.0140(12) 0.0079(10) 0.0009(10) 0.0073(10)
C17 0.0260(13) 0.0121(12) 0.0182(12) 0.0072(10) -0.0041(10) 0.0013(10)
C18 0.0168(12) 0.0165(12) 0.0255(13) 0.0150(11) 0.0013(10) 0.0000(10)
C19 0.0212(12) 0.0152(12) 0.0175(12) 0.0098(10) 0.0051(10) 0.0020(10)
C20 0.0181(12) 0.0150(12) 0.0222(13) 0.0086(10) 0.0039(10) 0.0007(10)
C21 0.0152(11) 0.0107(11) 0.0178(12) 0.0059(9) -0.0011(9) -0.0020(9)
C22 0.0171(12) 0.0170(12) 0.0193(12) 0.0094(10) 0.0013(10) 0.0074(10)
C23 0.0194(12) 0.0159(12) 0.0230(13) 0.0089(10) 0.0025(10) 0.0065(10)
C24 0.0234(13) 0.0313(15) 0.0290(15) 0.0211(13) 0.0072(11) 0.0130(11)
C25 0.0303(15) 0.0327(15) 0.0154(13) 0.0077(11) 0.0017(11) 0.0186(12)
C26 0.0284(14) 0.0170(13) 0.0244(14) 0.0033(11) -0.0057(11) 0.0089(11)
C27 0.0230(13) 0.0173(13) 0.0301(15) 0.0134(11) 0.0002(11) 0.0053(10)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C5 1.335(3) . ?
F2 C6 1.345(3) . ?
F3 C7 1.341(3) . ?
F4 C8 1.335(3) . ?
F5 C9 1.335(3) . ?
F6 C14 1.342(3) . ?
F7 C15 1.344(3) . ?
F8 C16 1.339(3) . ?
F9 C17 1.337(3) . ?
F10 C18 1.342(3) . ?
F11 C23 1.342(3) . ?
F12 C24 1.344(3) . ?
F13 C25 1.335(3) . ?
F14 C26 1.343(3) . ?
F15 C27 1.345(3) . ?
O1 C3 1.240(3) . ?
O2 C12 1.235(3) . ?
O3 C21 1.232(3) . ?
N1 C10 1.462(3) . ?
N1 C19 1.467(3) . ?
N1 C1 1.471(3) . ?
N2 C3 1.330(3) . ?
N2 C2 1.451(3) . ?
N2 H2C 0.86(3) . ?
N3 C3 1.376(3) . ?
N3 C4 1.404(3) . ?
N3 H3C 0.86(3) . ?
N4 C12 1.333(3) . ?
N4 C11 1.452(3) . ?
N4 H4C 0.85(3) . ?
N5 C12 1.376(3) . ?
N5 C13 1.394(3) . ?
N5 H5C 0.86(3) . ?
N6 C21 1.337(3) . ?
N6 C20 1.454(3) . ?
N6 H6C 0.85(3) . ?
N7 C21 1.391(3) . ?
N7 C22 1.394(3) . ?
N7 H7C 0.81(3) . ?
C1 C2 1.507(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 C5 1.386(3) . ?
C4 C9 1.389(3) . ?
C5 C6 1.382(3) . ?
C6 C7 1.370(4) . ?
C7 C8 1.374(4) . ?
C8 C9 1.388(4) . ?
C10 C11 1.514(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C18 1.389(3) . ?
C13 C14 1.389(3) . ?
C14 C15 1.375(3) . ?
C15 C16 1.373(3) . ?
C16 C17 1.379(3) . ?
C17 C18 1.377(3) . ?
C19 C20 1.511(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C22 C23 1.391(3) . ?
C22 C27 1.391(3) . ?
C23 C24 1.373(4) . ?
C24 C25 1.380(4) . ?
C25 C26 1.375(4) . ?
C26 C27 1.373(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
C10 N1 C19 111.94(18) . . ?
C10 N1 C1 112.20(18) . . ?
C19 N1 C1 111.35(18) . . ?
C3 N2 C2 121.2(2) . . ?
C3 N2 H2C 117.7(19) . . ?
C2 N2 H2C 120.8(19) . . ?
C3 N3 C4 121.7(2) . . ?
C3 N3 H3C 121.7(17) . . ?
C4 N3 H3C 115.4(17) . . ?
C12 N4 C11 122.4(2) . . ?
C12 N4 H4C 119(2) . . ?
C11 N4 H4C 118(2) . . ?
C12 N5 C13 122.9(2) . . ?
C12 N5 H5C 118(2) . . ?
C13 N5 H5C 118(2) . . ?
C21 N6 C20 123.9(2) . . ?
C21 N6 H6C 121.1(18) . . ?
C20 N6 H6C 114.8(18) . . ?
C21 N7 C22 122.7(2) . . ?
C21 N7 H7C 115.9(19) . . ?
C22 N7 H7C 116.6(19) . . ?
N1 C1 C2 112.01(19) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 C1 109.6(2) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
O1 C3 N2 123.7(2) . . ?
O1 C3 N3 120.8(2) . . ?
N2 C3 N3 115.5(2) . . ?
C5 C4 C9 117.1(2) . . ?
C5 C4 N3 121.4(2) . . ?
C9 C4 N3 121.5(2) . . ?
F1 C5 C6 118.4(2) . . ?
F1 C5 C4 120.0(2) . . ?
C6 C5 C4 121.6(2) . . ?
F2 C6 C7 120.2(2) . . ?
F2 C6 C5 119.6(2) . . ?
C7 C6 C5 120.1(2) . . ?
F3 C7 C6 120.4(2) . . ?
F3 C7 C8 119.7(2) . . ?
C6 C7 C8 119.9(2) . . ?
F4 C8 C7 120.3(2) . . ?
F4 C8 C9 120.0(2) . . ?
C7 C8 C9 119.7(2) . . ?
F5 C9 C8 118.4(2) . . ?
F5 C9 C4 120.0(2) . . ?
C8 C9 C4 121.6(2) . . ?
N1 C10 C11 112.50(19) . . ?
N1 C10 H10A 109.1 . . ?
C11 C10 H10A 109.1 . . ?
N1 C10 H10B 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N4 C11 C10 109.60(19) . . ?
N4 C11 H11A 109.8 . . ?
C10 C11 H11A 109.8 . . ?
N4 C11 H11B 109.8 . . ?
C10 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
O2 C12 N4 123.8(2) . . ?
O2 C12 N5 122.3(2) . . ?
N4 C12 N5 113.9(2) . . ?
C18 C13 C14 116.3(2) . . ?
C18 C13 N5 122.9(2) . . ?
C14 C13 N5 120.7(2) . . ?
F6 C14 C15 118.6(2) . . ?
F6 C14 C13 118.9(2) . . ?
C15 C14 C13 122.5(2) . . ?
F7 C15 C16 119.6(2) . . ?
F7 C15 C14 120.6(2) . . ?
C16 C15 C14 119.8(2) . . ?
F8 C16 C15 121.0(2) . . ?
F8 C16 C17 119.5(2) . . ?
C15 C16 C17 119.5(2) . . ?
F9 C17 C18 120.4(2) . . ?
F9 C17 C16 119.5(2) . . ?
C18 C17 C16 120.0(2) . . ?
F10 C18 C17 117.6(2) . . ?
F10 C18 C13 120.3(2) . . ?
C17 C18 C13 122.0(2) . . ?
N1 C19 C20 111.68(19) . . ?
N1 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
N1 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
N6 C20 C19 111.9(2) . . ?
N6 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 . . ?
N6 C20 H20B 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
O3 C21 N6 125.2(2) . . ?
O3 C21 N7 121.9(2) . . ?
N6 C21 N7 112.9(2) . . ?
C23 C22 C27 116.2(2) . . ?
C23 C22 N7 123.8(2) . . ?
C27 C22 N7 120.0(2) . . ?
F11 C23 C24 118.0(2) . . ?
F11 C23 C22 120.3(2) . . ?
C24 C23 C22 121.7(2) . . ?
F12 C24 C23 119.9(2) . . ?
F12 C24 C25 119.6(2) . . ?
C23 C24 C25 120.5(2) . . ?
F13 C25 C26 120.7(3) . . ?
F13 C25 C24 120.1(3) . . ?
C26 C25 C24 119.1(2) . . ?
F14 C26 C27 120.6(3) . . ?
F14 C26 C25 119.6(2) . . ?
C27 C26 C25 119.7(2) . . ?
F15 C27 C26 118.4(2) . . ?
F15 C27 C22 118.9(2) . . ?
C26 C27 C22 122.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.910
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.910
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.066


data_104psm
_database_code_depnum_ccdc_archive 'CCDC 655560'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H63 F15 N9 O8 P'
_chemical_formula_weight         1186.02

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           TRICLINIC
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.3363(11)
_cell_length_b                   14.0385(11)
_cell_length_c                   15.5942(13)
_cell_angle_alpha                99.391(2)
_cell_angle_beta                 95.841(2)
_cell_angle_gamma                108.885(2)
_cell_volume                     2687.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCKS
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9452
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_process_details   BRUKER-SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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 SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19376
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9400
_reflns_number_gt                7282
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SMART'
_computing_cell_refinement       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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 w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+1.1879P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9400
_refine_ls_number_parameters     750
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.1343
_refine_ls_wR_factor_gt          0.1252
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.03912(6) 0.51113(6) 0.13045(5) 0.0154(2) Uani 1 d . . .
F1 F -0.08696(14) 0.10677(13) 0.04998(12) 0.0247(4) Uani 1 d . . .
F2 F -0.13357(15) 0.00796(14) -0.11976(12) 0.0321(5) Uani 1 d . . .
F3 F -0.24803(16) 0.06634(15) -0.24098(12) 0.0367(5) Uani 1 d . . .
F4 F -0.32714(16) 0.22006(15) -0.18912(13) 0.0378(5) Uani 1 d . . .
F5 F -0.28860(15) 0.31309(14) -0.01773(13) 0.0317(5) Uani 1 d . . .
F6 F 0.44340(15) 0.55078(14) 0.29305(11) 0.0288(5) Uani 1 d . . .
F7 F 0.63239(15) 0.68615(14) 0.27535(14) 0.0377(5) Uani 1 d . . .
F8 F 0.66614(16) 0.73071(15) 0.11568(15) 0.0421(6) Uani 1 d . . .
F9 F 0.51001(16) 0.63583(14) -0.02778(13) 0.0342(5) Uani 1 d . . .
F10 F 0.32368(15) 0.49365(14) -0.01137(11) 0.0265(5) Uani 1 d . . .
F11 F -0.07741(15) 0.66206(14) 0.35111(12) 0.0318(5) Uani 1 d . . .
F12 F -0.10771(17) 0.84387(16) 0.38267(14) 0.0408(6) Uani 1 d . . .
F13 F 0.06515(19) 1.02165(15) 0.43044(14) 0.0458(6) Uani 1 d . . .
F14 F 0.26705(18) 1.01383(15) 0.44763(14) 0.0467(6) Uani 1 d . . .
F15 F 0.29699(15) 0.83293(15) 0.41455(13) 0.0370(5) Uani 1 d . . .
O1 O -0.21752(17) 0.13260(17) 0.17889(14) 0.0234(5) Uani 1 d . . .
O2 O 0.34366(16) 0.33584(16) 0.20406(14) 0.0205(5) Uani 1 d . . .
O3 O 0.21616(17) 0.65629(16) 0.49700(13) 0.0225(5) Uani 1 d . . .
O4 O 0.9710(2) 0.74726(18) 0.18173(15) 0.0331(6) Uani 1 d . . .
O5 O 0.04308(16) 0.46782(16) 0.21147(13) 0.0187(5) Uani 1 d . . .
O6 O -0.08204(16) 0.47894(16) 0.08860(14) 0.0172(5) Uani 1 d . . .
O7 O 0.10209(17) 0.47719(18) 0.06401(14) 0.0252(6) Uani 1 d . . .
O8 O 0.08496(19) 0.63148(18) 0.15465(16) 0.0264(6) Uani 1 d . . .
N1 N 0.0877(2) 0.28919(19) 0.35781(16) 0.0180(6) Uani 1 d . . .
N2 N -0.1135(2) 0.2933(2) 0.25633(18) 0.0209(6) Uani 1 d . . .
N3 N -0.1634(2) 0.2673(2) 0.10797(17) 0.0199(6) Uani 1 d . . .
N4 N 0.1651(2) 0.3109(2) 0.18871(17) 0.0174(6) Uani 1 d . . .
N5 N 0.2792(2) 0.4499(2) 0.14856(18) 0.0181(6) Uani 1 d . . .
N6 N 0.1756(2) 0.5135(2) 0.38853(19) 0.0240(7) Uani 1 d . . .
N7 N 0.1225(2) 0.6456(2) 0.36311(19) 0.0250(7) Uani 1 d . . .
N8 N 0.53428(19) 0.19488(18) 0.29859(15) 0.0134(6) Uani 1 d . . .
N9 N 0.8948(2) 0.8353(2) 0.10310(17) 0.0206(6) Uani 1 d . . .
C1 C -0.0204(2) 0.2168(3) 0.3565(2) 0.0232(8) Uani 1 d . . .
H1A H -0.0233 0.1944 0.4121 0.028 Uiso 1 calc R . .
H1B H -0.0351 0.1567 0.3100 0.028 Uiso 1 calc R . .
C2 C -0.1063(3) 0.2643(3) 0.3415(2) 0.0237(8) Uani 1 d . . .
H2A H -0.1753 0.2155 0.3459 0.028 Uiso 1 calc R . .
H2B H -0.0909 0.3249 0.3876 0.028 Uiso 1 calc R . .
C3 C -0.1672(2) 0.2238(2) 0.1817(2) 0.0184(7) Uani 1 d . . .
C4 C -0.1902(2) 0.2108(2) 0.0218(2) 0.0203(7) Uani 1 d . . .
C5 C -0.1514(2) 0.1331(2) -0.0066(2) 0.0177(7) Uani 1 d . . .
C6 C -0.1727(3) 0.0838(2) -0.0939(2) 0.0219(8) Uani 1 d . . .
C7 C -0.2305(3) 0.1129(3) -0.1558(2) 0.0252(8) Uani 1 d . . .
C8 C -0.2700(3) 0.1905(3) -0.1295(2) 0.0241(8) Uani 1 d . . .
C9 C -0.2498(3) 0.2372(2) -0.0426(2) 0.0217(8) Uani 1 d . . .
C10 C 0.1582(2) 0.2375(2) 0.3226(2) 0.0191(7) Uani 1 d . . .
H10A H 0.1445 0.1727 0.3418 0.023 Uiso 1 calc R . .
H10B H 0.2326 0.2801 0.3452 0.023 Uiso 1 calc R . .
C11 C 0.1395(3) 0.2173(2) 0.2225(2) 0.0187(7) Uani 1 d . . .
H11A H 0.1833 0.1784 0.2006 0.022 Uiso 1 calc R . .
H11B H 0.0648 0.1756 0.2004 0.022 Uiso 1 calc R . .
C12 C 0.2678(2) 0.3641(2) 0.18319(19) 0.0145(7) Uani 1 d . . .
C13 C 0.3790(2) 0.5174(2) 0.1409(2) 0.0167(7) Uani 1 d . . .
C14 C 0.4594(3) 0.5682(2) 0.2126(2) 0.0192(7) Uani 1 d . . .
C15 C 0.5555(3) 0.6386(3) 0.2047(2) 0.0263(8) Uani 1 d . . .
C16 C 0.5723(3) 0.6613(2) 0.1241(2) 0.0271(8) Uani 1 d . . .
C17 C 0.4934(3) 0.6132(3) 0.0514(2) 0.0236(8) Uani 1 d . . .
C18 C 0.3989(2) 0.5422(2) 0.0607(2) 0.0187(7) Uani 1 d . . .
C19 C 0.1351(3) 0.3544(3) 0.4449(2) 0.0234(8) Uani 1 d . . .
H19A H 0.1677 0.3180 0.4803 0.028 Uiso 1 calc R . .
H19B H 0.0790 0.3688 0.4739 0.028 Uiso 1 calc R . .
C20 C 0.2197(3) 0.4552(2) 0.4393(2) 0.0238(8) Uani 1 d . . .
H20A H 0.2502 0.4959 0.4983 0.029 Uiso 1 calc R . .
H20B H 0.2771 0.4407 0.4124 0.029 Uiso 1 calc R . .
C21 C 0.1753(3) 0.6075(2) 0.4223(2) 0.0197(7) Uani 1 d . . .
C22 C 0.1100(3) 0.7410(2) 0.3838(2) 0.0208(7) Uani 1 d . . .
C23 C 0.0090(3) 0.7483(2) 0.3765(2) 0.0228(8) Uani 1 d . . .
C24 C -0.0073(3) 0.8405(3) 0.3918(2) 0.0262(8) Uani 1 d . . .
C25 C 0.0799(3) 0.9310(3) 0.4168(2) 0.0294(9) Uani 1 d . . .
C26 C 0.1815(3) 0.9260(3) 0.4256(2) 0.0286(9) Uani 1 d . . .
C27 C 0.1963(3) 0.8329(3) 0.4093(2) 0.0243(8) Uani 1 d . . .
C28 C 0.6278(2) 0.2952(2) 0.3087(2) 0.0154(7) Uani 1 d . . .
H28A H 0.6763 0.3043 0.3625 0.019 Uiso 1 calc R . .
H28B H 0.6666 0.2884 0.2601 0.019 Uiso 1 calc R . .
C29 C 0.6000(2) 0.3919(2) 0.3115(2) 0.0175(7) Uani 1 d . . .
H29A H 0.5758 0.4091 0.3666 0.021 Uiso 1 calc R . .
H29B H 0.5425 0.3807 0.2635 0.021 Uiso 1 calc R . .
C30 C 0.6998(2) 0.4801(2) 0.3033(2) 0.0191(7) Uani 1 d . . .
H30A H 0.6911 0.5449 0.3261 0.023 Uiso 1 calc R . .
H30B H 0.7618 0.4769 0.3395 0.023 Uiso 1 calc R . .
C31 C 0.7216(3) 0.4782(3) 0.2099(2) 0.0270(8) Uani 1 d . . .
H31A H 0.7334 0.4155 0.1876 0.041 Uiso 1 calc R . .
H31B H 0.7842 0.5359 0.2093 0.041 Uiso 1 calc R . .
H31C H 0.6609 0.4819 0.1736 0.041 Uiso 1 calc R . .
C32 C 0.5852(2) 0.1153(2) 0.3125(2) 0.0167(7) Uani 1 d . . .
H32A H 0.6267 0.1363 0.3714 0.020 Uiso 1 calc R . .
H32B H 0.6351 0.1156 0.2713 0.020 Uiso 1 calc R . .
C33 C 0.5081(3) 0.0056(2) 0.3014(2) 0.0208(7) Uani 1 d . . .
H33A H 0.4840 -0.0250 0.2391 0.025 Uiso 1 calc R . .
H33B H 0.4456 0.0062 0.3281 0.025 Uiso 1 calc R . .
C34 C 0.5633(3) -0.0587(3) 0.3448(2) 0.0278(8) Uani 1 d . . .
H34A H 0.5826 -0.0299 0.4076 0.033 Uiso 1 calc R . .
H34B H 0.5124 -0.1280 0.3369 0.033 Uiso 1 calc R . .
C35 C 0.6629(3) -0.0643(3) 0.3094(3) 0.0373(10) Uani 1 d . . .
H35A H 0.6452 -0.0919 0.2471 0.056 Uiso 1 calc R . .
H35B H 0.6909 -0.1081 0.3381 0.056 Uiso 1 calc R . .
H35C H 0.7161 0.0034 0.3206 0.056 Uiso 1 calc R . .
C36 C 0.4608(2) 0.2043(2) 0.3650(2) 0.0171(7) Uani 1 d . . .
H36A H 0.4349 0.2598 0.3565 0.021 Uiso 1 calc R . .
H36B H 0.3989 0.1412 0.3522 0.021 Uiso 1 calc R . .
C37 C 0.5100(3) 0.2244(2) 0.4609(2) 0.0196(7) Uani 1 d . . .
H37A H 0.5810 0.2765 0.4716 0.024 Uiso 1 calc R . .
H37B H 0.5173 0.1618 0.4748 0.024 Uiso 1 calc R . .
C38 C 0.4389(3) 0.2608(2) 0.5205(2) 0.0219(8) Uani 1 d . . .
H38A H 0.3655 0.2132 0.5034 0.026 Uiso 1 calc R . .
H38B H 0.4632 0.2595 0.5810 0.026 Uiso 1 calc R . .
C39 C 0.4410(3) 0.3684(2) 0.5158(2) 0.0250(8) Uani 1 d . . .
H39A H 0.5132 0.4161 0.5341 0.037 Uiso 1 calc R . .
H39B H 0.3953 0.3873 0.5540 0.037 Uiso 1 calc R . .
H39C H 0.4157 0.3699 0.4563 0.037 Uiso 1 calc R . .
C40 C 0.4645(2) 0.1663(2) 0.20893(19) 0.0164(7) Uani 1 d . . .
H40A H 0.4283 0.2159 0.2067 0.020 Uiso 1 calc R . .
H40B H 0.4094 0.0998 0.2044 0.020 Uiso 1 calc R . .
C41 C 0.5188(2) 0.1608(2) 0.12810(19) 0.0166(7) Uani 1 d . . .
H41A H 0.5614 0.1167 0.1307 0.020 Uiso 1 calc R . .
H41B H 0.5657 0.2289 0.1251 0.020 Uiso 1 calc R . .
C42 C 0.4300(2) 0.1170(2) 0.0474(2) 0.0206(7) Uani 1 d . . .
H42A H 0.3854 0.0482 0.0510 0.025 Uiso 1 calc R . .
H42B H 0.3850 0.1592 0.0487 0.025 Uiso 1 calc R . .
C43 C 0.4714(3) 0.1119(3) -0.0396(2) 0.0243(8) Uani 1 d . . .
H43A H 0.5068 0.1804 -0.0477 0.036 Uiso 1 calc R . .
H43B H 0.4122 0.0763 -0.0869 0.036 Uiso 1 calc R . .
H43C H 0.5213 0.0756 -0.0394 0.036 Uiso 1 calc R . .
C44 C 0.8495(3) 0.8450(3) 0.0182(2) 0.0365(9) Uani 1 d . . .
H44A H 0.8947 0.9066 0.0034 0.055 Uiso 1 calc R . .
H44B H 0.7790 0.8483 0.0205 0.055 Uiso 1 calc R . .
H44C H 0.8447 0.7864 -0.0257 0.055 Uiso 1 calc R . .
C45 C 0.9003(3) 0.9120(3) 0.1799(2) 0.0328(9) Uani 1 d . . .
H45A H 0.8441 0.8836 0.2121 0.049 Uiso 1 calc R . .
H45B H 0.8916 0.9712 0.1613 0.049 Uiso 1 calc R . .
H45C H 0.9687 0.9320 0.2170 0.049 Uiso 1 calc R . .
C46 C 0.9295(3) 0.7591(2) 0.1117(2) 0.0236(8) Uani 1 d . . .
H46 H 0.9222 0.7104 0.0610 0.028 Uiso 1 calc R . .
H2C H -0.071(3) 0.347(2) 0.250(2) 0.016(9) Uiso 1 d . . .
H5C H 0.225(3) 0.452(2) 0.121(2) 0.021(10) Uiso 1 d . . .
H6C H 0.144(3) 0.487(3) 0.337(2) 0.025(10) Uiso 1 d . . .
H6D H -0.087(2) 0.494(2) 0.035(2) 0.020(9) Uiso 1 d . . .
H4C H 0.124(2) 0.341(2) 0.1889(19) 0.007(8) Uiso 1 d . . .
H7C H 0.092(3) 0.604(3) 0.315(2) 0.030(10) Uiso 1 d . . .
H3C H -0.142(3) 0.336(3) 0.115(2) 0.046(12) Uiso 1 d . . .
H8D H 0.041(3) 0.661(3) 0.163(3) 0.052(14) Uiso 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0148(4) 0.0191(5) 0.0138(4) 0.0045(3) 0.0013(3) 0.0076(4)
F1 0.0265(11) 0.0246(11) 0.0261(11) 0.0043(8) 0.0009(8) 0.0144(9)
F2 0.0372(12) 0.0278(11) 0.0319(12) -0.0012(9) 0.0102(10) 0.0145(10)
F3 0.0354(12) 0.0417(13) 0.0187(11) -0.0008(9) 0.0011(9) -0.0016(10)
F4 0.0373(12) 0.0363(12) 0.0315(12) 0.0133(10) -0.0141(10) 0.0046(10)
F5 0.0324(12) 0.0216(11) 0.0407(12) 0.0030(9) -0.0073(9) 0.0145(9)
F6 0.0342(12) 0.0299(11) 0.0187(10) 0.0047(9) -0.0036(9) 0.0087(9)
F7 0.0294(12) 0.0246(11) 0.0492(14) 0.0032(10) -0.0117(10) 0.0036(10)
F8 0.0283(12) 0.0265(12) 0.0703(16) 0.0146(11) 0.0167(11) 0.0032(10)
F9 0.0477(13) 0.0287(11) 0.0353(12) 0.0147(9) 0.0248(10) 0.0163(10)
F10 0.0338(11) 0.0280(11) 0.0199(10) 0.0049(8) 0.0036(9) 0.0141(9)
F11 0.0265(11) 0.0305(12) 0.0301(11) 0.0074(9) -0.0036(9) 0.0010(9)
F12 0.0416(13) 0.0533(14) 0.0419(13) 0.0175(11) 0.0117(11) 0.0305(12)
F13 0.0819(18) 0.0271(12) 0.0415(13) 0.0129(10) 0.0220(12) 0.0301(12)
F14 0.0548(15) 0.0217(12) 0.0455(14) 0.0022(10) 0.0017(11) -0.0065(11)
F15 0.0241(12) 0.0413(13) 0.0412(13) 0.0100(10) 0.0024(10) 0.0057(10)
O1 0.0247(13) 0.0200(13) 0.0267(13) 0.0081(10) 0.0072(10) 0.0068(11)
O2 0.0169(12) 0.0200(12) 0.0268(13) 0.0053(10) 0.0014(10) 0.0096(10)
O3 0.0244(13) 0.0239(13) 0.0142(12) -0.0020(10) -0.0029(10) 0.0064(11)
O4 0.0514(17) 0.0302(14) 0.0238(14) 0.0070(11) 0.0038(12) 0.0223(13)
O5 0.0173(12) 0.0206(12) 0.0162(12) 0.0028(9) -0.0018(9) 0.0057(10)
O6 0.0187(12) 0.0217(12) 0.0129(12) 0.0055(10) 0.0016(9) 0.0087(10)
O7 0.0205(12) 0.0482(15) 0.0188(12) 0.0131(11) 0.0068(10) 0.0236(12)
O8 0.0187(13) 0.0211(13) 0.0362(15) 0.0060(11) -0.0038(11) 0.0053(11)
N1 0.0166(14) 0.0209(15) 0.0174(14) 0.0055(12) 0.0024(11) 0.0069(12)
N2 0.0165(16) 0.0238(17) 0.0213(16) 0.0056(14) 0.0024(12) 0.0054(14)
N3 0.0242(16) 0.0145(15) 0.0193(15) 0.0020(12) 0.0014(12) 0.0058(13)
N4 0.0164(15) 0.0185(15) 0.0220(16) 0.0066(12) 0.0057(12) 0.0105(13)
N5 0.0122(15) 0.0215(16) 0.0237(16) 0.0094(13) 0.0031(12) 0.0078(13)
N6 0.0300(17) 0.0270(17) 0.0148(16) 0.0004(13) -0.0054(13) 0.0141(14)
N7 0.0360(18) 0.0219(16) 0.0144(16) -0.0040(13) -0.0069(14) 0.0136(14)
N8 0.0120(13) 0.0106(13) 0.0155(14) 0.0012(11) -0.0003(11) 0.0027(11)
N9 0.0222(15) 0.0216(15) 0.0188(15) 0.0040(12) 0.0026(12) 0.0091(13)
C1 0.0232(19) 0.0267(19) 0.0217(18) 0.0116(15) 0.0081(15) 0.0070(16)
C2 0.0178(18) 0.031(2) 0.0206(18) 0.0048(15) 0.0064(14) 0.0061(16)
C3 0.0137(17) 0.0237(19) 0.0229(18) 0.0056(15) 0.0053(14) 0.0121(15)
C4 0.0155(17) 0.0211(18) 0.0224(18) 0.0051(15) 0.0040(14) 0.0034(15)
C5 0.0125(16) 0.0212(18) 0.0187(17) 0.0067(14) 0.0009(13) 0.0042(14)
C6 0.0196(18) 0.0182(18) 0.0256(19) 0.0026(15) 0.0083(15) 0.0031(15)
C7 0.0217(19) 0.0252(19) 0.0185(19) 0.0014(15) 0.0016(15) -0.0035(16)
C8 0.0179(18) 0.0224(19) 0.026(2) 0.0108(16) -0.0055(15) -0.0013(15)
C9 0.0185(18) 0.0137(17) 0.030(2) 0.0046(15) -0.0013(15) 0.0030(14)
C10 0.0169(17) 0.0180(17) 0.0261(19) 0.0091(15) 0.0036(14) 0.0087(14)
C11 0.0181(17) 0.0149(17) 0.0211(18) 0.0027(14) 0.0037(14) 0.0034(14)
C12 0.0170(18) 0.0168(17) 0.0105(16) 0.0003(13) 0.0009(13) 0.0083(14)
C13 0.0181(18) 0.0151(17) 0.0225(18) 0.0040(14) 0.0033(14) 0.0134(14)
C14 0.0223(18) 0.0185(17) 0.0217(18) 0.0060(14) 0.0054(15) 0.0121(15)
C15 0.0198(19) 0.0212(19) 0.035(2) 0.0029(16) -0.0026(16) 0.0075(16)
C16 0.024(2) 0.0170(18) 0.046(2) 0.0138(17) 0.0152(18) 0.0093(16)
C17 0.033(2) 0.0223(19) 0.028(2) 0.0112(16) 0.0169(17) 0.0185(17)
C18 0.0173(18) 0.0208(18) 0.0220(18) 0.0041(15) 0.0027(14) 0.0124(15)
C19 0.0221(19) 0.032(2) 0.0200(18) 0.0088(15) 0.0019(15) 0.0131(16)
C20 0.0230(19) 0.028(2) 0.0206(18) 0.0033(15) -0.0051(15) 0.0130(16)
C21 0.0180(18) 0.0216(18) 0.0167(18) 0.0029(15) 0.0020(14) 0.0040(15)
C22 0.028(2) 0.0195(18) 0.0143(17) 0.0036(14) 0.0023(14) 0.0075(16)
C23 0.027(2) 0.0207(19) 0.0152(17) 0.0050(14) 0.0000(15) 0.0014(16)
C24 0.036(2) 0.031(2) 0.0188(18) 0.0092(16) 0.0059(16) 0.0190(18)
C25 0.051(3) 0.0195(19) 0.0208(19) 0.0052(15) 0.0077(17) 0.0159(19)
C26 0.036(2) 0.0195(19) 0.0207(19) 0.0037(15) 0.0049(16) -0.0034(17)
C27 0.025(2) 0.027(2) 0.0182(18) 0.0051(15) 0.0022(15) 0.0065(16)
C28 0.0116(16) 0.0152(17) 0.0180(17) 0.0032(13) 0.0002(13) 0.0035(13)
C29 0.0171(17) 0.0171(17) 0.0181(17) 0.0012(14) 0.0025(14) 0.0069(14)
C30 0.0193(18) 0.0184(17) 0.0196(17) 0.0035(14) 0.0044(14) 0.0064(14)
C31 0.032(2) 0.0220(19) 0.028(2) 0.0053(15) 0.0106(16) 0.0094(16)
C32 0.0172(17) 0.0181(17) 0.0192(17) 0.0056(14) 0.0030(14) 0.0110(14)
C33 0.0212(18) 0.0163(17) 0.0270(19) 0.0059(15) 0.0034(15) 0.0085(15)
C34 0.031(2) 0.0217(19) 0.035(2) 0.0117(16) 0.0054(17) 0.0113(16)
C35 0.040(2) 0.035(2) 0.047(2) 0.0126(19) 0.0110(19) 0.025(2)
C36 0.0175(17) 0.0151(17) 0.0227(18) 0.0041(14) 0.0079(14) 0.0094(14)
C37 0.0222(18) 0.0161(17) 0.0236(18) 0.0060(14) 0.0061(14) 0.0089(15)
C38 0.0231(19) 0.0213(18) 0.0207(18) 0.0028(14) 0.0067(15) 0.0069(15)
C39 0.031(2) 0.0271(19) 0.0186(18) 0.0017(15) 0.0027(15) 0.0144(17)
C40 0.0153(17) 0.0136(16) 0.0189(17) 0.0024(13) -0.0009(13) 0.0049(14)
C41 0.0146(16) 0.0160(17) 0.0198(17) 0.0029(13) 0.0017(13) 0.0071(14)
C42 0.0179(17) 0.0206(18) 0.0209(18) 0.0032(14) 0.0007(14) 0.0048(15)
C43 0.0255(19) 0.027(2) 0.0193(18) 0.0047(15) -0.0010(15) 0.0091(16)
C44 0.038(2) 0.048(3) 0.029(2) 0.0119(18) 0.0007(17) 0.021(2)
C45 0.040(2) 0.032(2) 0.030(2) 0.0027(17) 0.0071(17) 0.0186(18)
C46 0.0256(19) 0.0187(18) 0.0217(19) -0.0011(15) 0.0039(15) 0.0040(15)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O5 1.492(2) . ?
P1 O7 1.510(2) . ?
P1 O8 1.564(2) . ?
P1 O6 1.568(2) . ?
F1 C5 1.346(3) . ?
F2 C6 1.353(4) . ?
F3 C7 1.342(4) . ?
F4 C8 1.343(3) . ?
F5 C9 1.348(4) . ?
F6 C14 1.342(3) . ?
F7 C15 1.341(4) . ?
F8 C16 1.348(4) . ?
F9 C17 1.346(4) . ?
F10 C18 1.345(3) . ?
F11 C23 1.341(4) . ?
F12 C24 1.349(4) . ?
F13 C25 1.336(4) . ?
F14 C26 1.346(4) . ?
F15 C27 1.337(4) . ?
O1 C3 1.229(4) . ?
O2 C12 1.233(3) . ?
O3 C21 1.221(4) . ?
O4 C46 1.234(4) . ?
O6 H6D 0.89(3) . ?
O8 H8D 0.83(4) . ?
N1 C19 1.459(4) . ?
N1 C10 1.460(4) . ?
N1 C1 1.466(4) . ?
N2 C3 1.352(4) . ?
N2 C2 1.454(4) . ?
N2 H2C 0.81(3) . ?
N3 C3 1.385(4) . ?
N3 C4 1.391(4) . ?
N3 H3C 0.89(4) . ?
N4 C12 1.351(4) . ?
N4 C11 1.447(4) . ?
N4 H4C 0.79(3) . ?
N5 C12 1.369(4) . ?
N5 C13 1.391(4) . ?
N5 H5C 0.81(3) . ?
N6 C21 1.340(4) . ?
N6 C20 1.439(4) . ?
N6 H6C 0.84(3) . ?
N7 C21 1.381(4) . ?
N7 C22 1.392(4) . ?
N7 H7C 0.84(3) . ?
N8 C40 1.514(4) . ?
N8 C36 1.515(4) . ?
N8 C32 1.515(4) . ?
N8 C28 1.521(4) . ?
N9 C46 1.317(4) . ?
N9 C44 1.444(4) . ?
N9 C45 1.452(4) . ?
C1 C2 1.516(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 C5 1.382(4) . ?
C4 C9 1.388(4) . ?
C5 C6 1.377(4) . ?
C6 C7 1.370(5) . ?
C7 C8 1.379(5) . ?
C8 C9 1.364(4) . ?
C10 C11 1.521(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C18 1.382(4) . ?
C13 C14 1.382(4) . ?
C14 C15 1.373(4) . ?
C15 C16 1.369(5) . ?
C16 C17 1.377(5) . ?
C17 C18 1.369(4) . ?
C19 C20 1.520(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C22 C23 1.378(4) . ?
C22 C27 1.388(4) . ?
C23 C24 1.369(5) . ?
C24 C25 1.380(5) . ?
C25 C26 1.374(5) . ?
C26 C27 1.372(5) . ?
C28 C29 1.513(4) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.530(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.511(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.520(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.531(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.509(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.514(4) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.536(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.516(4) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 C41 1.520(4) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.528(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.516(4) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 P1 O7 113.78(12) . . ?
O5 P1 O8 110.51(13) . . ?
O7 P1 O8 107.25(14) . . ?
O5 P1 O6 107.55(12) . . ?
O7 P1 O6 110.62(12) . . ?
O8 P1 O6 106.93(12) . . ?
P1 O6 H6D 110(2) . . ?
P1 O8 H8D 117(3) . . ?
C19 N1 C10 112.0(2) . . ?
C19 N1 C1 112.1(2) . . ?
C10 N1 C1 112.2(2) . . ?
C3 N2 C2 121.9(3) . . ?
C3 N2 H2C 116(2) . . ?
C2 N2 H2C 120(2) . . ?
C3 N3 C4 124.0(3) . . ?
C3 N3 H3C 119(2) . . ?
C4 N3 H3C 117(2) . . ?
C12 N4 C11 120.4(3) . . ?
C12 N4 H4C 117(2) . . ?
C11 N4 H4C 119(2) . . ?
C12 N5 C13 122.5(3) . . ?
C12 N5 H5C 116(2) . . ?
C13 N5 H5C 120(2) . . ?
C21 N6 C20 123.0(3) . . ?
C21 N6 H6C 117(2) . . ?
C20 N6 H6C 120(2) . . ?
C21 N7 C22 123.1(3) . . ?
C21 N7 H7C 115(2) . . ?
C22 N7 H7C 122(2) . . ?
C40 N8 C36 105.6(2) . . ?
C40 N8 C32 112.0(2) . . ?
C36 N8 C32 111.5(2) . . ?
C40 N8 C28 111.3(2) . . ?
C36 N8 C28 111.3(2) . . ?
C32 N8 C28 105.4(2) . . ?
C46 N9 C44 121.6(3) . . ?
C46 N9 C45 120.4(3) . . ?
C44 N9 C45 118.1(3) . . ?
N1 C1 C2 112.2(3) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 C1 113.1(3) . . ?
N2 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
O1 C3 N2 124.4(3) . . ?
O1 C3 N3 123.0(3) . . ?
N2 C3 N3 112.6(3) . . ?
C5 C4 C9 116.3(3) . . ?
C5 C4 N3 122.8(3) . . ?
C9 C4 N3 120.7(3) . . ?
F1 C5 C6 117.9(3) . . ?
F1 C5 C4 120.5(3) . . ?
C6 C5 C4 121.5(3) . . ?
F2 C6 C7 119.2(3) . . ?
F2 C6 C5 120.2(3) . . ?
C7 C6 C5 120.6(3) . . ?
F3 C7 C6 120.1(3) . . ?
F3 C7 C8 120.7(3) . . ?
C6 C7 C8 119.2(3) . . ?
F4 C8 C9 120.5(3) . . ?
F4 C8 C7 120.2(3) . . ?
C9 C8 C7 119.3(3) . . ?
F5 C9 C8 118.8(3) . . ?
F5 C9 C4 118.2(3) . . ?
C8 C9 C4 123.0(3) . . ?
N1 C10 C11 110.6(2) . . ?
N1 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N4 C11 C10 112.8(2) . . ?
N4 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
N4 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
O2 C12 N4 123.1(3) . . ?
O2 C12 N5 123.2(3) . . ?
N4 C12 N5 113.7(3) . . ?
C18 C13 C14 116.7(3) . . ?
C18 C13 N5 120.4(3) . . ?
C14 C13 N5 122.7(3) . . ?
F6 C14 C15 118.3(3) . . ?
F6 C14 C13 119.7(3) . . ?
C15 C14 C13 122.0(3) . . ?
F7 C15 C16 119.7(3) . . ?
F7 C15 C14 120.6(3) . . ?
C16 C15 C14 119.6(3) . . ?
F8 C16 C15 120.1(3) . . ?
F8 C16 C17 119.9(3) . . ?
C15 C16 C17 120.0(3) . . ?
F9 C17 C18 120.8(3) . . ?
F9 C17 C16 119.9(3) . . ?
C18 C17 C16 119.3(3) . . ?
F10 C18 C17 118.7(3) . . ?
F10 C18 C13 119.0(3) . . ?
C17 C18 C13 122.3(3) . . ?
N1 C19 C20 111.5(3) . . ?
N1 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
N1 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
N6 C20 C19 111.9(3) . . ?
N6 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 . . ?
N6 C20 H20B 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
O3 C21 N6 125.2(3) . . ?
O3 C21 N7 122.1(3) . . ?
N6 C21 N7 112.7(3) . . ?
C23 C22 C27 116.5(3) . . ?
C23 C22 N7 120.6(3) . . ?
C27 C22 N7 122.9(3) . . ?
F11 C23 C24 118.1(3) . . ?
F11 C23 C22 119.2(3) . . ?
C24 C23 C22 122.7(3) . . ?
F12 C24 C23 120.6(3) . . ?
F12 C24 C25 119.7(3) . . ?
C23 C24 C25 119.7(3) . . ?
F13 C25 C26 120.8(3) . . ?
F13 C25 C24 120.3(3) . . ?
C26 C25 C24 118.9(3) . . ?
F14 C26 C27 120.0(3) . . ?
F14 C26 C25 119.4(3) . . ?
C27 C26 C25 120.6(3) . . ?
F15 C27 C26 118.0(3) . . ?
F15 C27 C22 120.3(3) . . ?
C26 C27 C22 121.6(3) . . ?
C29 C28 N8 116.7(2) . . ?
C29 C28 H28A 108.1 . . ?
N8 C28 H28A 108.1 . . ?
C29 C28 H28B 108.1 . . ?
N8 C28 H28B 108.1 . . ?
H28A C28 H28B 107.3 . . ?
C28 C29 C30 109.0(2) . . ?
C28 C29 H29A 109.9 . . ?
C30 C29 H29A 109.9 . . ?
C28 C29 H29B 109.9 . . ?
C30 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
C31 C30 C29 113.7(3) . . ?
C31 C30 H30A 108.8 . . ?
C29 C30 H30A 108.8 . . ?
C31 C30 H30B 108.8 . . ?
C29 C30 H30B 108.8 . . ?
H30A C30 H30B 107.7 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 C33 115.9(2) . . ?
N8 C32 H32A 108.3 . . ?
C33 C32 H32A 108.3 . . ?
N8 C32 H32B 108.3 . . ?
C33 C32 H32B 108.3 . . ?
H32A C32 H32B 107.4 . . ?
C32 C33 C34 110.4(3) . . ?
C32 C33 H33A 109.6 . . ?
C34 C33 H33A 109.6 . . ?
C32 C33 H33B 109.6 . . ?
C34 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
C35 C34 C33 114.6(3) . . ?
C35 C34 H34A 108.6 . . ?
C33 C34 H34A 108.6 . . ?
C35 C34 H34B 108.6 . . ?
C33 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 N8 116.0(2) . . ?
C37 C36 H36A 108.3 . . ?
N8 C36 H36A 108.3 . . ?
C37 C36 H36B 108.3 . . ?
N8 C36 H36B 108.3 . . ?
H36A C36 H36B 107.4 . . ?
C36 C37 C38 110.3(3) . . ?
C36 C37 H37A 109.6 . . ?
C38 C37 H37A 109.6 . . ?
C36 C37 H37B 109.6 . . ?
C38 C37 H37B 109.6 . . ?
H37A C37 H37B 108.1 . . ?
C39 C38 C37 112.9(3) . . ?
C39 C38 H38A 109.0 . . ?
C37 C38 H38A 109.0 . . ?
C39 C38 H38B 109.0 . . ?
C37 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N8 C40 C41 117.8(2) . . ?
N8 C40 H40A 107.9 . . ?
C41 C40 H40A 107.9 . . ?
N8 C40 H40B 107.9 . . ?
C41 C40 H40B 107.9 . . ?
H40A C40 H40B 107.2 . . ?
C40 C41 C42 107.2(2) . . ?
C40 C41 H41A 110.3 . . ?
C42 C41 H41A 110.3 . . ?
C40 C41 H41B 110.3 . . ?
C42 C41 H41B 110.3 . . ?
H41A C41 H41B 108.5 . . ?
C43 C42 C41 113.8(3) . . ?
C43 C42 H42A 108.8 . . ?
C41 C42 H42A 108.8 . . ?
C43 C42 H42B 108.8 . . ?
C41 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N9 C44 H44A 109.5 . . ?
N9 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N9 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N9 C45 H45A 109.5 . . ?
N9 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N9 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O4 C46 N9 125.0(3) . . ?
O4 C46 H46 117.5 . . ?
N9 C46 H46 117.5 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.060