 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2001-02-26 at 14:03:56
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.1
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : s92
 
 
data_s92
 
_audit_creation_date            2001-02-26T14:03:56-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.1
_audit_conform_dict_location    ftp://ftp.iucr.org/cifdics/cif_core.dic
_publ_requested_category        FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_sum                   'C46 H64 N6 O14 P6'
_chemical_formula_weight                1110.85
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_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                          10.255(2)
_cell_length_b                          11.320(2)
_cell_length_c                          12.800(3)
_cell_angle_alpha                       83.74(3)
_cell_angle_beta                        72.10(3)
_cell_angle_gamma                       66.53(3)
_cell_volume                            1296.8(5)
_cell_formula_units_Z                   1
_cell_measurement_temperature           150(2)
_cell_measurement_reflns_used           7119
_cell_measurement_theta_min             2.91
_cell_measurement_theta_max             27.48
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              block
_exptl_crystal_colour                   colourless
_exptl_crystal_size_max                 0.28
_exptl_crystal_size_mid                 0.16
_exptl_crystal_size_min                 0.1
_exptl_crystal_density_diffrn           1.422
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    584
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.278
_exptl_absorpt_correction_T_min         0.9263
_exptl_absorpt_correction_T_max         0.9728
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_ambient_temperature             150(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_reflns_number                   19041
_diffrn_reflns_av_R_equivalents         0.1016
_diffrn_reflns_av_unetI/netI            0.0822
_diffrn_reflns_limit_h_min              -12
_diffrn_reflns_limit_h_max              13
_diffrn_reflns_limit_k_min              -14
_diffrn_reflns_limit_k_max              14
_diffrn_reflns_limit_l_min              -16
_diffrn_reflns_limit_l_max              16
_diffrn_reflns_theta_min                3.18
_diffrn_reflns_theta_max                27.44
_diffrn_reflns_theta_full               27.44
_diffrn_measured_fraction_theta_full
                                        0.988
_diffrn_measured_fraction_theta_max
                                        0.988
_reflns_number_total                    5869
_reflns_number_gt                       4608
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0938P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            SHELXL
_refine_ls_extinction_expression
                                    Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef              0.011(3)
_refine_ls_number_reflns                5869
_refine_ls_number_parameters            454
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0718
_refine_ls_R_factor_gt                  0.0534
_refine_ls_wR_factor_ref                0.146
_refine_ls_wR_factor_gt                 0.134
_refine_ls_goodness_of_fit_ref          1.012
_refine_ls_restrained_S_all             1.012
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.489
_refine_diff_density_min                -0.739
_refine_diff_density_rms                0.104
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
 
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 0.2741(2) 0.0682(2) 0.35973(16) 0.0178(4) Uani 1 1 d . . .
C2 C 0.4166(2) 0.0135(2) 0.37364(19) 0.0233(5) Uani 1 1 d . . .
C3 C 0.4666(3) -0.1085(2) 0.4171(2) 0.0285(5) Uani 1 1 d . . .
C4 C 0.3755(3) -0.1771(3) 0.4477(2) 0.0314(6) Uani 1 1 d . . .
C5 C 0.2342(3) -0.1234(2) 0.4349(2) 0.0302(6) Uani 1 1 d . . .
C6 C 0.1837(3) -0.0015(2) 0.39135(19) 0.0237(5) Uani 1 1 d . . .
C7 C 0.2682(2) 0.3232(2) 0.35745(17) 0.0169(4) Uani 1 1 d . . .
C8 C 0.3983(2) 0.3439(2) 0.30798(19) 0.0213(5) Uani 1 1 d . . .
C9 C 0.4374(3) 0.4210(2) 0.3608(2) 0.0275(5) Uani 1 1 d . . .
C10 C 0.3460(3) 0.4764(2) 0.4624(2) 0.0278(5) Uani 1 1 d . . .
C11 C 0.2163(3) 0.4567(2) 0.5114(2) 0.0251(5) Uani 1 1 d . . .
C12 C 0.1779(2) 0.3793(2) 0.45921(18) 0.0192(5) Uani 1 1 d . . .
C13 C -0.1786(3) 0.1221(2) 0.2218(2) 0.0222(5) Uani 1 1 d . . .
C14 C -0.1911(3) 0.0001(2) 0.2723(2) 0.0267(5) Uani 1 1 d . . .
C15 C -0.0435(3) -0.2060(2) 0.3186(2) 0.0278(5) Uani 1 1 d . . .
C16 C 0.1025(3) -0.3154(2) 0.27632(19) 0.0272(5) Uani 1 1 d . . .
C17 C 0.2419(3) -0.4367(2) 0.1080(2) 0.0293(5) Uani 1 1 d . . .
C18 C 0.2865(4) -0.3481(3) 0.0215(2) 0.0333(6) Uani 1 1 d . . .
C19 C 0.3171(3) -0.1491(2) 0.00941(19) 0.0273(5) Uani 1 1 d . . .
C20 C 0.3231(3) -0.0572(2) 0.08107(18) 0.0202(5) Uani 1 1 d . . .
C21 C 0.2662(3) 0.2649(2) -0.13012(17) 0.0208(5) Uani 1 1 d . . .
C22 C -0.1465(2) 0.5002(2) 0.16552(19) 0.0192(5) Uani 1 1 d . . .
C23 C -0.2841(3) 0.6212(2) 0.19873(18) 0.0226(5) Uani 1 1 d . . .
N1 N 0.06606(19) 0.22347(18) 0.11340(14) 0.0185(4) Uani 1 1 d . . .
N2 N 0.03772(18) 0.28129(17) 0.32086(14) 0.0158(4) Uani 1 1 d . . .
N3 N 0.30870(18) 0.20498(18) 0.16624(14) 0.0175(4) Uani 1 1 d . . .
O1 O -0.11745(16) 0.17171(14) 0.28613(12) 0.0188(3) Uani 1 1 d . . .
O2 O -0.04725(17) -0.09793(15) 0.25004(13) 0.0280(4) Uani 1 1 d . . .
O3 O 0.09981(18) -0.37115(17) 0.18295(14) 0.0310(4) Uani 1 1 d . . .
O4 O 0.32167(18) -0.26224(16) 0.07059(13) 0.0277(4) Uani 1 1 d . . .
O5 O 0.32470(16) 0.05527(14) 0.01626(11) 0.0190(3) Uani 1 1 d . . .
O6 O 0.28164(16) 0.27924(14) -0.02310(11) 0.0185(3) Uani 1 1 d . . .
O7 O -0.17575(15) 0.39488(14) 0.23033(12) 0.0179(3) Uani 1 1 d . . .
P1 P 0.21556(6) 0.22203(5) 0.29326(4) 0.01469(16) Uani 1 1 d . . .
P2 P -0.03701(6) 0.26659(5) 0.23458(4) 0.01450(16) Uani 1 1 d . . .
P3 P 0.23946(6) 0.19196(5) 0.07537(4) 0.01511(16) Uani 1 1 d . . .
H2 H 0.479(3) 0.062(3) 0.352(2) 0.032(7) Uiso 1 1 d . . .
H3 H 0.562(3) -0.143(3) 0.428(2) 0.033(7) Uiso 1 1 d . . .
H4 H 0.405(3) -0.258(3) 0.472(2) 0.030(7) Uiso 1 1 d . . .
H5 H 0.166(3) -0.171(3) 0.464(2) 0.033(7) Uiso 1 1 d . . .
H6 H 0.082(3) 0.039(2) 0.382(2) 0.025(6) Uiso 1 1 d . . .
H8 H 0.464(3) 0.307(2) 0.240(2) 0.022(6) Uiso 1 1 d . . .
H9 H 0.527(3) 0.441(3) 0.329(2) 0.042(8) Uiso 1 1 d . . .
H10 H 0.369(3) 0.536(3) 0.494(2) 0.030(7) Uiso 1 1 d . . .
H11 H 0.152(4) 0.500(3) 0.579(3) 0.061(10) Uiso 1 1 d . . .
H12 H 0.098(3) 0.363(3) 0.492(2) 0.029(7) Uiso 1 1 d . . .
H131 H -0.268(3) 0.186(3) 0.221(2) 0.030(7) Uiso 1 1 d . . .
H132 H -0.118(3) 0.107(2) 0.145(2) 0.017(6) Uiso 1 1 d . . .
H141 H -0.250(3) -0.030(3) 0.241(2) 0.040(8) Uiso 1 1 d . . .
H142 H -0.237(3) 0.013(3) 0.354(2) 0.034(7) Uiso 1 1 d . . .
H151 H -0.131(3) -0.236(3) 0.321(2) 0.032(7) Uiso 1 1 d . . .
H152 H -0.056(3) -0.182(3) 0.397(3) 0.044(8) Uiso 1 1 d . . .
H161 H 0.187(3) -0.284(2) 0.257(2) 0.022(6) Uiso 1 1 d . . .
H162 H 0.119(3) -0.383(2) 0.333(2) 0.025(6) Uiso 1 1 d . . .
H171 H 0.232(3) -0.505(3) 0.071(2) 0.026(6) Uiso 1 1 d . . .
H172 H 0.321(3) -0.477(3) 0.151(3) 0.056(9) Uiso 1 1 d . . .
H181 H 0.376(3) -0.402(3) -0.038(2) 0.041(8) Uiso 1 1 d . . .
H182 H 0.201(3) -0.297(3) -0.002(2) 0.041(8) Uiso 1 1 d . . .
H191 H 0.403(3) -0.167(3) -0.056(3) 0.043(8) Uiso 1 1 d . . .
H192 H 0.221(3) -0.108(3) -0.016(2) 0.043(8) Uiso 1 1 d . . .
H201 H 0.237(3) -0.034(3) 0.144(2) 0.029(7) Uiso 1 1 d . . .
H202 H 0.412(3) -0.091(3) 0.106(2) 0.028(7) Uiso 1 1 d . . .
H211 H 0.345(3) 0.183(3) -0.161(2) 0.024(6) Uiso 1 1 d . . .
H212 H 0.165(3) 0.267(2) -0.1165(19) 0.017(6) Uiso 1 1 d . . .
H221 H -0.123(3) 0.481(2) 0.094(2) 0.025(7) Uiso 1 1 d . . .
H222 H -0.055(3) 0.510(3) 0.182(2) 0.030(7) Uiso 1 1 d . . .
H231 H -0.376(3) 0.604(2) 0.192(2) 0.022(6) Uiso 1 1 d . . .
H232 H -0.301(3) 0.644(3) 0.274(2) 0.030(7) Uiso 1 1 d . . .
 
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_distance
    _geom_bond_site_symmetry_2
    _geom_bond_publ_flag
C1 C6 1.389(3) . ?
C1 C2 1.402(3) . ?
C1 P1 1.810(2) . ?
C2 C3 1.386(3) . ?
C3 C4 1.384(4) . ?
C4 C5 1.385(4) . ?
C5 C6 1.387(3) . ?
C7 C12 1.389(3) . ?
C7 C8 1.390(3) . ?
C7 P1 1.803(2) . ?
C8 C9 1.398(3) . ?
C9 C10 1.386(4) . ?
C10 C11 1.381(4) . ?
C11 C12 1.390(3) . ?
C13 O1 1.444(3) . ?
C13 C14 1.495(3) . ?
C14 O2 1.413(3) . ?
C15 O2 1.420(3) . ?
C15 C16 1.496(4) . ?
C16 O3 1.423(3) . ?
C17 O3 1.425(3) . ?
C17 C18 1.501(3) . ?
C18 O4 1.422(3) . ?
C19 O4 1.418(3) . ?
C19 C20 1.490(3) . ?
C20 O5 1.445(3) . ?
C21 O6 1.460(3) . ?
C21 C23 1.520(3) 2_565 ?
C22 O7 1.455(2) . ?
C22 C23 1.505(3) . ?
C23 C21 1.520(3) 2_565 ?
N1 P2 1.5836(19) . ?
N1 P3 1.5896(18) . ?
N2 P2 1.5801(17) . ?
N2 P1 1.6068(18) . ?
N3 P3 1.5834(18) . ?
N3 P1 1.5999(18) . ?
O1 P2 1.5767(15) . ?
O5 P3 1.5819(17) . ?
O6 P3 1.5765(15) . ?
O7 P2 1.5877(16) . ?
 
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle_publ_flag
C6 C1 C2 118.8(2) . . ?
C6 C1 P1 121.09(16) . . ?
C2 C1 P1 120.00(16) . . ?
C3 C2 C1 120.4(2) . . ?
C4 C3 C2 120.1(2) . . ?
C3 C4 C5 119.8(2) . . ?
C4 C5 C6 120.4(2) . . ?
C5 C6 C1 120.5(2) . . ?
C12 C7 C8 119.8(2) . . ?
C12 C7 P1 118.97(16) . . ?
C8 C7 P1 121.25(18) . . ?
C7 C8 C9 119.9(2) . . ?
C10 C9 C8 119.7(2) . . ?
C11 C10 C9 120.5(2) . . ?
C10 C11 C12 119.8(2) . . ?
C7 C12 C11 120.4(2) . . ?
O1 C13 C14 108.62(19) . . ?
O2 C14 C13 108.61(19) . . ?
O2 C15 C16 109.26(19) . . ?
O3 C16 C15 108.6(2) . . ?
O3 C17 C18 111.6(2) . . ?
O4 C18 C17 108.6(2) . . ?
O4 C19 C20 107.46(18) . . ?
O5 C20 C19 106.86(17) . . ?
O6 C21 C23 107.30(18) . 2_565 ?
O7 C22 C23 108.12(17) . . ?
C22 C23 C21 111.59(19) . 2_565 ?
P2 N1 P3 123.60(11) . . ?
P2 N2 P1 119.77(11) . . ?
P3 N3 P1 120.97(11) . . ?
C13 O1 P2 120.86(13) . . ?
C14 O2 C15 112.12(18) . . ?
C16 O3 C17 114.87(19) . . ?
C19 O4 C18 113.70(18) . . ?
C20 O5 P3 118.39(13) . . ?
C21 O6 P3 120.32(13) . . ?
C22 O7 P2 117.53(13) . . ?
N3 P1 N2 116.87(10) . . ?
N3 P1 C7 108.10(10) . . ?
N2 P1 C7 108.35(10) . . ?
N3 P1 C1 108.97(10) . . ?
N2 P1 C1 109.16(10) . . ?
C7 P1 C1 104.72(9) . . ?
O1 P2 N2 106.48(9) . . ?
O1 P2 N1 111.34(9) . . ?
N2 P2 N1 117.54(9) . . ?
O1 P2 O7 100.46(8) . . ?
N2 P2 O7 110.58(9) . . ?
N1 P2 O7 109.09(10) . . ?
O6 P3 O5 99.87(8) . . ?
O6 P3 N3 106.86(9) . . ?
O5 P3 N3 111.92(9) . . ?
O6 P3 N1 111.33(9) . . ?
O5 P3 N1 109.07(9) . . ?
N3 P3 N1 116.52(10) . . ?
 
