 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2001-12-13 at 09:09:38
#  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  : ljf068 dreduc struct gaussian sortav
 
 
data_ljf068
 
_audit_creation_date            2001-12-13T09:09:38-00:00
_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        FM
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C12 H30 Cl4 P2 Pd2'
_chemical_formula_sum                   'C12 H30 Cl4 P2 Pd2'
_chemical_formula_weight                590.9
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 1 21/n 1'
_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                          7.45460(10)
_cell_length_b                          12.1561(2)
_cell_length_c                          12.0156(2)
_cell_angle_alpha                       90
_cell_angle_beta                        101.8090(10)
_cell_angle_gamma                       90
_cell_volume                            1065.79(3)
_cell_formula_units_Z                   2
_cell_measurement_temperature           100(2)
_cell_measurement_reflns_used           4561
_cell_measurement_theta_min             2
_cell_measurement_theta_max             34.972
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   orange
_exptl_crystal_size_max                 0.31
_exptl_crystal_size_mid                 0.2
_exptl_crystal_size_min                 0.15
_exptl_crystal_density_diffrn           1.841
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    584
loop_
    _exptl_crystal_face_index_h
    _exptl_crystal_face_index_k
    _exptl_crystal_face_index_l
    _exptl_crystal_face_perp_dist
0 1 1 0.07
0 -1 -1 0.08
0 -1 1 0.1
0 1 -1 0.1
1 0 -1 0.11
-1 0 1 0.2
 
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           2.329
_exptl_absorpt_correction_type          gaussian
_exptl_absorpt_process_details
;
   P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_absorpt_correction_T_min         0.518
_exptl_absorpt_correction_T_max         0.806
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             100(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             0.716544E-1
_diffrn_orient_matrix_ub_12             -0.605745E-1
_diffrn_orient_matrix_ub_13             -0.266423E-1
_diffrn_orient_matrix_ub_21             0.444623E-1
_diffrn_orient_matrix_ub_22             0.524649E-1
_diffrn_orient_matrix_ub_23             -0.52493E-1
_diffrn_orient_matrix_ub_31             0.108029
_diffrn_orient_matrix_ub_32             0.18585E-1
_diffrn_orient_matrix_ub_33             0.613504E-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         0.0332
_diffrn_reflns_av_unetI/netI            0.0224
_diffrn_reflns_number                   20457
_diffrn_reflns_limit_h_min              -11
_diffrn_reflns_limit_h_max              12
_diffrn_reflns_limit_k_min              -19
_diffrn_reflns_limit_k_max              16
_diffrn_reflns_limit_l_min              -19
_diffrn_reflns_limit_l_max              19
_diffrn_reflns_theta_min                3.26
_diffrn_reflns_theta_max                35.03
_diffrn_reflns_theta_full               35.03
_diffrn_measured_fraction_theta_full
                                        0.991
_diffrn_measured_fraction_theta_max
                                        0.991
_reflns_number_total                    4649
_reflns_number_gt                       4417
_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)+(0.0119P)²+0.6284P] 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              0.0054(4)
_refine_ls_number_reflns                4649
_refine_ls_number_parameters            95
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0199
_refine_ls_R_factor_gt                  0.0182
_refine_ls_wR_factor_ref                0.0429
_refine_ls_wR_factor_gt                 0.0422
_refine_ls_goodness_of_fit_ref          1.082
_refine_ls_restrained_S_all             1.082
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.595
_refine_diff_density_min                -0.906
_refine_diff_density_rms                0.086
 
#----------------------------------------------------------------------------#
#                   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
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
Pd Pd 0.105628(10) 0.101902(6) 0.094842(6) 0.01154(3) Uani 1 1 d . . .
Cl1 Cl -0.18942(3) 0.06738(2) -0.03171(2) 0.01693(5) Uani 1 1 d . . .
Cl2 Cl 0.00969(4) 0.26572(2) 0.15600(2) 0.01842(5) Uani 1 1 d . . .
P P 0.37745(4) 0.13607(2) 0.20560(2) 0.01355(5) Uani 1 1 d . . .
C11 C 0.54459(15) 0.02911(9) 0.19591(10) 0.01642(18) Uani 1 1 d . . .
H11A H 0.494 -0.0425 0.2139 0.02 Uiso 1 1 calc R . .
H11B H 0.5615 0.0255 0.1164 0.02 Uiso 1 1 calc R . .
C12 C 0.73246(16) 0.04496(11) 0.27422(11) 0.0223(2) Uani 1 1 d . . .
H12A H 0.786 0.1145 0.2557 0.033 Uiso 1 1 calc R . .
H12B H 0.8132 -0.016 0.2635 0.033 Uiso 1 1 calc R . .
H12C H 0.7184 0.0465 0.3535 0.033 Uiso 1 1 calc R . .
C21 C 0.36515(17) 0.14884(10) 0.35427(10) 0.0196(2) Uani 1 1 d . . .
H21A H 0.49 0.1619 0.3996 0.024 Uiso 1 1 calc R . .
H21B H 0.2893 0.2137 0.3636 0.024 Uiso 1 1 calc R . .
C22 C 0.28435(18) 0.04751(11) 0.40079(10) 0.0223(2) Uani 1 1 d . . .
H22A H 0.1579 0.0367 0.3595 0.033 Uiso 1 1 calc R . .
H22B H 0.2857 0.0581 0.4818 0.033 Uiso 1 1 calc R . .
H22C H 0.3576 -0.0173 0.3909 0.033 Uiso 1 1 calc R . .
C31 C 0.47257(17) 0.26568(10) 0.16900(12) 0.0231(2) Uani 1 1 d . . .
H31A H 0.4065 0.327 0.1971 0.028 Uiso 1 1 calc R . .
H31B H 0.6028 0.2701 0.2083 0.028 Uiso 1 1 calc R . .
C32 C 0.4602(2) 0.27999(13) 0.04149(14) 0.0324(3) Uani 1 1 d . . .
H32A H 0.5308 0.2218 0.0137 0.049 Uiso 1 1 calc R . .
H32B H 0.5102 0.3519 0.027 0.049 Uiso 1 1 calc R . .
H32C H 0.3317 0.2754 0.0019 0.049 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
Pd 0.01249(4) 0.01021(4) 0.01206(4) -0.00060(2) 0.00283(3) -0.00072(2)
Cl1 0.01444(10) 0.01438(10) 0.02066(11) -0.00493(9) 0.00052(8) 0.00150(8)
Cl2 0.01943(11) 0.01267(10) 0.02317(12) -0.00414(9) 0.00436(9) 0.00069(8)
P 0.01412(11) 0.01099(11) 0.01504(11) 0.00034(9) 0.00179(9) -0.00170(8)
C11 0.0153(4) 0.0156(4) 0.0179(4) 0.0012(3) 0.0023(3) 0.0003(3)
C12 0.0164(5) 0.0236(5) 0.0248(5) 0.0036(4) -0.0008(4) 0.0004(4)
C21 0.0234(5) 0.0184(5) 0.0158(5) -0.0045(4) 0.0014(4) -0.0002(4)
C22 0.0262(5) 0.0249(5) 0.0171(5) 0.0019(4) 0.0072(4) 0.0037(4)
C31 0.0180(5) 0.0143(4) 0.0357(7) 0.0068(4) 0.0028(4) -0.0034(4)
C32 0.0286(6) 0.0291(6) 0.0432(8) 0.0181(6) 0.0160(6) 0.0018(5)
 
 
#----------------------------------------------------------------------------#
#                   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
Pd P 2.2239(3) . ?
Pd Cl2 2.2875(3) . ?
Pd Cl1 2.3225(3) 3 ?
Pd Cl1 2.4407(3) . ?
Cl1 Pd 2.3225(3) 3 ?
P C21 1.8141(12) . ?
P C31 1.8183(12) . ?
P C11 1.8209(11) . ?
C11 C12 1.5311(16) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C21 C22 1.5265(18) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C31 C32 1.526(2) . ?
C31 H31A 0.99 . ?
C31 H31B 0.99 . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
 
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
P Pd Cl2 87.228(10) . . ?
P Pd Cl1 95.043(10) . 3 ?
Cl2 Pd Cl1 177.386(10) . 3 ?
P Pd Cl1 178.165(10) . . ?
Cl2 Pd Cl1 92.794(9) . . ?
Cl1 Pd Cl1 84.978(9) 3 . ?
Pd Cl1 Pd 95.022(9) 3 . ?
C21 P C31 105.36(6) . . ?
C21 P C11 107.29(5) . . ?
C31 P C11 107.30(6) . . ?
C21 P Pd 112.44(4) . . ?
C31 P Pd 111.70(4) . . ?
C11 P Pd 112.33(4) . . ?
C12 C11 P 115.00(8) . . ?
C12 C11 H11A 108.5 . . ?
P C11 H11A 108.5 . . ?
C12 C11 H11B 108.5 . . ?
P C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C22 C21 P 113.25(8) . . ?
C22 C21 H21A 108.9 . . ?
P C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
P C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C32 C31 P 113.28(10) . . ?
C32 C31 H31A 108.9 . . ?
P C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
P C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
 
