 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2001-06-26 at 16:19:22
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.2
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf049a dreduc sortav absorb struct
 
 
data_ljf049a
 
_audit_creation_date            2001-06-26T16:19:22-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.2
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category        FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C26 H17 F6 P'
_chemical_formula_structural            'C26 H17 F6 P'
_chemical_formula_sum                   'C26 H17 F6 P'
_chemical_formula_weight                474.37
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 21/n'
_symmetry_space_group_name_Hall         '-P 2yn'
_symmetry_Int_Tables_number             14
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                          15.3320(2)
_cell_length_b                          9.7078(1)
_cell_length_c                          16.1202(2)
_cell_angle_alpha                       90
_cell_angle_beta                        113.8367(6)
_cell_angle_gamma                       90
_cell_volume                            2194.67(5)
_cell_formula_units_Z                   4
_cell_measurement_temperature           150(2)
_cell_measurement_reflns_used           35353
_cell_measurement_theta_min             2
_cell_measurement_theta_max             30.034
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   'pale yellow'
_exptl_crystal_size_max                 0.5
_exptl_crystal_size_mid                 0.5
_exptl_crystal_size_min                 0.4
_exptl_crystal_density_diffrn           1.436
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    968
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.187
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min         0.93
_exptl_absorpt_correction_T_max         0.965
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             150(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_detector                        'CCD plate'
_diffrn_orient_matrix_type              'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11             0.54594E-1
_diffrn_orient_matrix_ub_12             -0.339336E-1
_diffrn_orient_matrix_ub_13             -0.132909E-1
_diffrn_orient_matrix_ub_21             -0.201343E-1
_diffrn_orient_matrix_ub_22             -0.972269E-1
_diffrn_orient_matrix_ub_23             0.28973E-2
_diffrn_orient_matrix_ub_31             -0.412135E-1
_diffrn_orient_matrix_ub_32             0.25483E-2
_diffrn_orient_matrix_ub_33             -0.664406E-1
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents         0.0404
_diffrn_reflns_av_unetI/netI            0.0164
_diffrn_reflns_number                   73044
_diffrn_reflns_limit_h_min              -20
_diffrn_reflns_limit_h_max              21
_diffrn_reflns_limit_k_min              -13
_diffrn_reflns_limit_k_max              13
_diffrn_reflns_limit_l_min              -22
_diffrn_reflns_limit_l_max              22
_diffrn_reflns_theta_min                2.37
_diffrn_reflns_theta_max                30.06
_diffrn_reflns_theta_full               30.06
_diffrn_measured_fraction_theta_full
                                        0.998
_diffrn_measured_fraction_theta_max
                                        0.998
_reflns_number_total                    6430
_reflns_number_gt                       5677
_reflns_threshold_expression            >2sigma(I)
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement
                                       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
                             'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution           'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0427P)²+0.8816P] 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            none
_refine_ls_number_reflns                6430
_refine_ls_number_parameters            298
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0427
_refine_ls_R_factor_gt                  0.0353
_refine_ls_wR_factor_ref                0.0933
_refine_ls_wR_factor_gt                 0.0897
_refine_ls_goodness_of_fit_ref          1.023
_refine_ls_restrained_S_all             1.023
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.34
_refine_diff_density_min                -0.304
_refine_diff_density_rms                0.043
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
loop_
    _atom_site_label
    _atom_site_type_symbol
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_occupancy
    _atom_site_symmetry_multiplicity
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_disorder_assembly
    _atom_site_disorder_group
P1 P 0.572210(19) 0.64176(3) 0.184133(18) 0.02311(7) Uani 1 1 d . . .
F1 F 0.25067(6) 0.43990(9) 0.31215(5) 0.04122(19) Uani 1 1 d . . .
F2 F 0.32936(6) 0.37673(8) 0.23457(6) 0.0447(2) Uani 1 1 d . . .
F3 F 0.21866(6) 0.52807(10) 0.18065(6) 0.0500(2) Uani 1 1 d . . .
F4 F 0.49138(8) 0.87650(8) 0.55094(6) 0.0480(2) Uani 1 1 d . . .
F5 F 0.47561(7) 0.66361(9) 0.57665(5) 0.0445(2) Uani 1 1 d . . .
F6 F 0.60310(6) 0.73333(11) 0.56591(5) 0.0499(2) Uani 1 1 d . . .
C1 C 0.48885(7) 0.87538(11) 0.22491(7) 0.02203(19) Uani 1 1 d . . .
C2 C 0.46686(8) 1.01514(11) 0.22263(7) 0.0260(2) Uani 1 1 d . . .
H2 H 0.4339 1.0483 0.2574 0.031 Uiso 1 1 calc R . .
C3 C 0.49263(8) 1.10649(12) 0.16999(8) 0.0295(2) Uani 1 1 d . . .
H3 H 0.4769 1.2014 0.1684 0.035 Uiso 1 1 calc R . .
C4 C 0.54138(8) 1.05852(12) 0.11985(8) 0.0296(2) Uani 1 1 d . . .
H4 H 0.5582 1.1203 0.083 0.036 Uiso 1 1 calc R . .
C5 C 0.56585(8) 0.91979(12) 0.12336(7) 0.0263(2) Uani 1 1 d . . .
H5 H 0.6004 0.8882 0.0896 0.032 Uiso 1 1 calc R . .
C6 C 0.54041(7) 0.82622(11) 0.17569(7) 0.02228(19) Uani 1 1 d . . .
C7 C 0.45895(7) 0.78288(11) 0.28271(7) 0.02216(19) Uani 1 1 d . . .
C8 C 0.39139(7) 0.67906(11) 0.24482(7) 0.02380(19) Uani 1 1 d . . .
H8 H 0.3657 0.6633 0.1812 0.029 Uiso 1 1 calc R . .
C9 C 0.36153(7) 0.59861(11) 0.29989(7) 0.0241(2) Uani 1 1 d . . .
C10 C 0.39813(8) 0.61923(11) 0.39322(7) 0.0251(2) Uani 1 1 d . . .
H10 H 0.3775 0.5641 0.4306 0.03 Uiso 1 1 calc R . .
C11 C 0.46555(8) 0.72235(11) 0.43046(7) 0.02367(19) Uani 1 1 d . . .
C12 C 0.49590(7) 0.80358(11) 0.37611(7) 0.02341(19) Uani 1 1 d . . .
H12 H 0.5421 0.8736 0.4029 0.028 Uiso 1 1 calc R . .
C13 C 0.64728(8) 0.63319(11) 0.11977(7) 0.02389(19) Uani 1 1 d . . .
C14 C 0.60056(8) 0.61814(12) 0.02533(7) 0.0285(2) Uani 1 1 d . . .
H14 H 0.5329 0.6173 -0.0025 0.034 Uiso 1 1 calc R . .
C15 C 0.65221(9) 0.60444(12) -0.02794(8) 0.0309(2) Uani 1 1 d . . .
H15 H 0.6197 0.5945 -0.0918 0.037 Uiso 1 1 calc R . .
C16 C 0.75121(9) 0.60518(12) 0.01190(8) 0.0314(2) Uani 1 1 d . . .
H16 H 0.7866 0.5961 -0.0245 0.038 Uiso 1 1 calc R . .
C17 C 0.79811(9) 0.61929(12) 0.10541(8) 0.0306(2) Uani 1 1 d . . .
H17 H 0.8658 0.6193 0.133 0.037 Uiso 1 1 calc R . .
C18 C 0.74668(8) 0.63334(11) 0.15911(7) 0.0271(2) Uani 1 1 d . . .
H18 H 0.7796 0.6431 0.2229 0.032 Uiso 1 1 calc R . .
C19 C 0.65895(7) 0.63325(10) 0.30261(7) 0.02256(19) Uani 1 1 d . . .
C20 C 0.71351(8) 0.74552(11) 0.34977(8) 0.0279(2) Uani 1 1 d . . .
H20 H 0.7081 0.8313 0.3197 0.033 Uiso 1 1 calc R . .
C21 C 0.77566(9) 0.73274(13) 0.44040(8) 0.0325(2) Uani 1 1 d . . .
H21 H 0.8121 0.8099 0.472 0.039 Uiso 1 1 calc R . .
C22 C 0.78463(9) 0.60755(14) 0.48487(8) 0.0334(2) Uani 1 1 d . . .
H22 H 0.8271 0.599 0.5468 0.04 Uiso 1 1 calc R . .
C23 C 0.73156(9) 0.49543(13) 0.43864(8) 0.0342(3) Uani 1 1 d . . .
H23 H 0.7381 0.4095 0.4688 0.041 Uiso 1 1 calc R . .
C24 C 0.66857(8) 0.50801(12) 0.34806(8) 0.0286(2) Uani 1 1 d . . .
H24 H 0.6319 0.4308 0.317 0.034 Uiso 1 1 calc R . .
C25 C 0.29024(8) 0.48651(13) 0.25723(8) 0.0309(2) Uani 1 1 d . . .
C26 C 0.50863(9) 0.74836(12) 0.53067(8) 0.0293(2) Uani 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
P1 C19 1.8358(11) . ?
P1 C13 1.8367(11) . ?
P1 C6 1.8463(11) . ?
F1 C25 1.3382(13) . ?
F2 C25 1.3439(15) . ?
F3 C25 1.3403(14) . ?
F4 C26 1.3394(13) . ?
F5 C26 1.3363(13) . ?
F6 C26 1.3330(15) . ?
C1 C2 1.3949(15) . ?
C1 C6 1.4105(14) . ?
C1 C7 1.4933(14) . ?
C2 C3 1.3905(15) . ?
C2 H2 0.95 . ?
C3 C4 1.3845(17) . ?
C3 H3 0.95 . ?
C4 C5 1.3931(16) . ?
C4 H4 0.95 . ?
C5 C6 1.3981(14) . ?
C5 H5 0.95 . ?
C7 C12 1.3924(14) . ?
C7 C8 1.3966(15) . ?
C8 C9 1.3914(14) . ?
C8 H8 0.95 . ?
C9 C10 1.3914(15) . ?
C9 C25 1.4981(15) . ?
C10 C11 1.3890(15) . ?
C10 H10 0.95 . ?
C11 C12 1.3912(14) . ?
C11 C26 1.4991(15) . ?
C12 H12 0.95 . ?
C13 C18 1.3941(15) . ?
C13 C14 1.4039(15) . ?
C14 C15 1.3899(16) . ?
C14 H14 0.95 . ?
C15 C16 1.3886(18) . ?
C15 H15 0.95 . ?
C16 C17 1.3900(17) . ?
C16 H16 0.95 . ?
C17 C18 1.3932(16) . ?
C17 H17 0.95 . ?
C18 H18 0.95 . ?
C19 C24 1.3961(14) . ?
C19 C20 1.3971(15) . ?
C20 C21 1.3901(16) . ?
C20 H20 0.95 . ?
C21 C22 1.3894(18) . ?
C21 H21 0.95 . ?
C22 C23 1.3828(19) . ?
C22 H22 0.95 . ?
C23 C24 1.3928(17) . ?
C23 H23 0.95 . ?
C24 H24 0.95 . ?
 
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
C19 P1 C13 103.28(5) . . ?
C19 P1 C6 100.32(5) . . ?
C13 P1 C6 102.09(5) . . ?
C2 C1 C6 119.91(9) . . ?
C2 C1 C7 118.00(9) . . ?
C6 C1 C7 122.06(9) . . ?
C3 C2 C1 120.74(10) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C4 C3 C2 119.69(10) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.10(10) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 121.09(10) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 118.42(10) . . ?
C5 C6 P1 123.02(8) . . ?
C1 C6 P1 118.56(7) . . ?
C12 C7 C8 118.87(9) . . ?
C12 C7 C1 119.64(9) . . ?
C8 C7 C1 121.43(9) . . ?
C9 C8 C7 120.21(9) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 121.08(10) . . ?
C10 C9 C25 120.10(10) . . ?
C8 C9 C25 118.82(10) . . ?
C11 C10 C9 118.39(10) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
C10 C11 C12 121.08(9) . . ?
C10 C11 C26 120.93(9) . . ?
C12 C11 C26 117.98(10) . . ?
C11 C12 C7 120.37(10) . . ?
C11 C12 H12 119.8 . . ?
C7 C12 H12 119.8 . . ?
C18 C13 C14 118.57(10) . . ?
C18 C13 P1 124.23(8) . . ?
C14 C13 P1 117.11(8) . . ?
C15 C14 C13 120.76(11) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C16 C15 C14 120.20(10) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 119.46(11) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 120.58(11) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C17 C18 C13 120.43(10) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C24 C19 C20 118.74(10) . . ?
C24 C19 P1 117.62(8) . . ?
C20 C19 P1 123.62(8) . . ?
C21 C20 C19 120.51(10) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C20 120.21(11) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C21 119.77(11) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.24(11) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 120.53(11) . . ?
C23 C24 H24 119.7 . . ?
C19 C24 H24 119.7 . . ?
F1 C25 F3 106.84(10) . . ?
F1 C25 F2 106.45(10) . . ?
F3 C25 F2 106.12(10) . . ?
F1 C25 C9 112.57(10) . . ?
F3 C25 C9 112.22(10) . . ?
F2 C25 C9 112.20(9) . . ?
F6 C26 F5 106.64(10) . . ?
F6 C26 F4 106.59(10) . . ?
F5 C26 F4 106.26(9) . . ?
F6 C26 C11 111.74(9) . . ?
F5 C26 C11 113.15(10) . . ?
F4 C26 C11 112.01(10) . . ?
 
