#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/82/2008234.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2008234
loop_
_publ_author_name
'Cave, Gareth W. V.'
'Errington, William'
'Rourke, Jonathan P.'
_publ_section_title
;
 trans-Diiodobis(triphenylphosphine)palladium(II)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              320
_journal_page_last               322
_journal_paper_doi               10.1107/S0108270198015868
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Pd I2 (C18 H15 P1)2]'
_chemical_formula_moiety         'C36 H30 I2 P2 Pd'
_chemical_formula_sum            'C36 H30 I2 P2 Pd'
_chemical_formula_weight         884.74
_chemical_name_systematic
;
 trans-Diiodobis(triphenylphosphine)palladium(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.424(3)
_cell_angle_beta                 87.870(10)
_cell_angle_gamma                67.852(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3761(6)
_cell_length_b                   9.4407(5)
_cell_length_c                   10.7822(6)
_cell_measurement_reflns_used    3679
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.66
_cell_measurement_theta_min      2.00
_cell_volume                     834.18(9)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994a)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC (Siemens, 1994b)'
_computing_publication_material  'SHELXTL/PC (Siemens, 1994b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL/PC (Siemens, 1994b)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.842
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4960
_diffrn_reflns_theta_full        28.66
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.526
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.951
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.047
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0530P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.094
_reflns_number_gt                2793
_reflns_number_total             3608
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf1284.cif
_cod_data_source_block           cf1284
_cod_original_cell_volume        834.18(2)
_cod_database_code               2008234
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Pd1 0 0 0 0.01958(11) Uani d S 1 . . Pd
I1 0.23187(4) -0.19913(4) -0.07763(3) 0.03839(12) Uani d . 1 . . I
P1 -0.00861(12) 0.20600(13) -0.19581(10) 0.0219(2) Uani d . 1 . . P
C11 0.1824(5) 0.2069(5) -0.2350(5) 0.0283(9) Uani d . 1 . . C
C12 0.2284(6) 0.2280(6) -0.3607(5) 0.0355(11) Uani d . 1 . . C
H12A 0.1609 0.2401 -0.4302 0.043 Uiso calc R 1 . . H
C13 0.3747(6) 0.2315(7) -0.3849(6) 0.0505(15) Uani d . 1 . . C
H13A 0.4078 0.2440 -0.4707 0.061 Uiso calc R 1 . . H
C14 0.4706(6) 0.2167(7) -0.2843(7) 0.0521(16) Uani d . 1 . . C
H14A 0.5690 0.2217 -0.3013 0.063 Uiso calc R 1 . . H
C15 0.4260(6) 0.1950(7) -0.1605(7) 0.0530(15) Uani d . 1 . . C
H15A 0.4931 0.1854 -0.0918 0.064 Uiso calc R 1 . . H
C16 0.2827(6) 0.1867(7) -0.1342(5) 0.0413(12) Uani d . 1 . . C
H16A 0.2535 0.1671 -0.0469 0.050 Uiso calc R 1 . . H
C21 -0.0948(5) 0.1898(5) -0.3372(4) 0.0266(9) Uani d . 1 . . C
C22 -0.1153(5) 0.0486(6) -0.3264(5) 0.0300(10) Uani d . 1 . . C
H22A -0.0838 -0.0389 -0.2458 0.036 Uiso calc R 1 . . H
C23 -0.1811(5) 0.0342(6) -0.4318(5) 0.0386(12) Uani d . 1 . . C
H23A -0.1952 -0.0630 -0.4229 0.046 Uiso calc R 1 . . H
C24 -0.2264(6) 0.1587(8) -0.5494(5) 0.0475(14) Uani d . 1 . . C
H24A -0.2705 0.1477 -0.6220 0.057 Uiso calc R 1 . . H
C25 -0.2073(7) 0.2995(7) -0.5610(5) 0.0512(15) Uani d . 1 . . C
H25A -0.2386 0.3860 -0.6422 0.061 Uiso calc R 1 . . H
C26 -0.1432(6) 0.3172(6) -0.4562(5) 0.0414(12) Uani d . 1 . . C
H26A -0.1321 0.4159 -0.4652 0.050 Uiso calc R 1 . . H
C31 -0.1207(5) 0.4147(5) -0.2034(4) 0.0301(10) Uani d . 1 . . C
C32 -0.0526(7) 0.5067(6) -0.1699(5) 0.0435(13) Uani d . 1 . . C
H32A 0.0564 0.4657 -0.1512 0.052 Uiso calc R 1 . . H
C33 -0.1438(8) 0.6580(7) -0.1637(6) 0.0570(16) Uani d . 1 . . C
H33A -0.0964 0.7188 -0.1383 0.068 Uiso calc R 1 . . H
C34 -0.2999(8) 0.7219(7) -0.1932(6) 0.0579(17) Uani d . 1 . . C
H34A -0.3604 0.8272 -0.1906 0.069 Uiso calc R 1 . . H
C35 -0.3688(7) 0.6329(7) -0.2266(6) 0.0516(15) Uani d . 1 . . C
H35A -0.4780 0.6761 -0.2455 0.062 Uiso calc R 1 . . H
C36 -0.2817(6) 0.4808(6) -0.2332(5) 0.0402(12) Uani d . 1 . . C
H36A -0.3307 0.4210 -0.2580 0.048 Uiso calc R 1 . . H
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P1 Pd1 P1 2 . 180.00(5) ?
P1 Pd1 I1 2 2 88.45(3) ?
P1 Pd1 I1 . 2 91.55(3) ?
P1 Pd1 I1 2 . 91.55(3) ?
P1 Pd1 I1 . . 88.45(3) y
I1 Pd1 I1 2 . 180.000(13) ?
C31 P1 C21 . . 103.1(2) ?
C31 P1 C11 . . 103.1(2) ?
C21 P1 C11 . . 107.1(2) ?
C31 P1 Pd1 . . 117.26(15) ?
C21 P1 Pd1 . . 112.24(14) ?
C11 P1 Pd1 . . 112.90(15) ?
C12 C11 C16 . . 119.6(4) ?
C12 C11 P1 . . 122.5(4) ?
C16 C11 P1 . . 117.9(4) ?
C11 C12 C13 . . 119.7(5) ?
C14 C13 C12 . . 119.8(5) ?
C15 C14 C13 . . 120.7(5) ?
C14 C15 C16 . . 120.2(6) ?
C11 C16 C15 . . 120.0(5) ?
C22 C21 C26 . . 118.7(4) ?
C22 C21 P1 . . 119.5(3) ?
C26 C21 P1 . . 121.7(4) ?
C23 C22 C21 . . 120.5(5) ?
C24 C23 C22 . . 120.7(5) ?
C23 C24 C25 . . 119.3(5) ?
C26 C25 C24 . . 121.0(5) ?
C25 C26 C21 . . 119.8(5) ?
C32 C31 C36 . . 118.4(4) ?
C32 C31 P1 . . 121.6(4) ?
C36 C31 P1 . . 119.8(4) ?
C33 C32 C31 . . 119.9(5) ?
C34 C33 C32 . . 121.5(6) ?
C33 C34 C35 . . 119.4(5) ?
C34 C35 C36 . . 120.8(5) ?
C35 C36 C31 . . 120.0(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 P1 2 2.3504(10) ?
Pd1 P1 . 2.3504(10) y
Pd1 I1 2 2.5975(3) ?
Pd1 I1 . 2.5975(3) y
P1 C31 . 1.826(4) y
P1 C21 . 1.826(4) y
P1 C11 . 1.828(4) y
C11 C12 . 1.382(6) ?
C11 C16 . 1.382(7) ?
C12 C13 . 1.398(7) ?
C13 C14 . 1.373(9) ?
C14 C15 . 1.359(8) ?
C15 C16 . 1.389(7) ?
C21 C22 . 1.385(6) ?
C21 C26 . 1.396(6) ?
C22 C23 . 1.381(6) ?
C23 C24 . 1.373(8) ?
C24 C25 . 1.373(8) ?
C25 C26 . 1.383(7) ?
C31 C32 . 1.388(7) ?
C31 C36 . 1.403(7) ?
C32 C33 . 1.383(7) ?
C33 C34 . 1.362(9) ?
C34 C35 . 1.369(8) ?
C35 C36 . 1.382(7) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
P1 Pd1 P1 C31 2 -6E1(10)
I1 Pd1 P1 C31 2 15.14(18)
I1 Pd1 P1 C31 . -164.86(18)
P1 Pd1 P1 C21 2 18E1(10)
I1 Pd1 P1 C21 2 -103.99(15)
I1 Pd1 P1 C21 . 76.01(15)
P1 Pd1 P1 C11 2 6E1(10)
I1 Pd1 P1 C11 2 134.80(16)
I1 Pd1 P1 C11 . -45.20(16)
C31 P1 C11 C12 . -95.7(4)
C21 P1 C11 C12 . 12.8(4)
Pd1 P1 C11 C12 . 136.8(3)
C31 P1 C11 C16 . 83.9(4)
C21 P1 C11 C16 . -167.7(4)
Pd1 P1 C11 C16 . -43.6(4)
C16 C11 C12 C13 . -1.1(7)
P1 C11 C12 C13 . 178.4(4)
C11 C12 C13 C14 . -1.1(8)
C12 C13 C14 C15 . 1.5(9)
C13 C14 C15 C16 . 0.3(9)
C12 C11 C16 C15 . 2.9(8)
P1 C11 C16 C15 . -176.6(4)
C14 C15 C16 C11 . -2.6(8)
C31 P1 C21 C22 . -140.8(4)
C11 P1 C21 C22 . 110.8(4)
Pd1 P1 C21 C22 . -13.7(4)
C31 P1 C21 C26 . 38.2(4)
C11 P1 C21 C26 . -70.2(4)
Pd1 P1 C21 C26 . 165.4(3)
C26 C21 C22 C23 . 0.5(7)
P1 C21 C22 C23 . 179.6(3)
C21 C22 C23 C24 . 0.5(7)
C22 C23 C24 C25 . -0.8(8)
C23 C24 C25 C26 . 0.0(8)
C24 C25 C26 C21 . 1.0(8)
C22 C21 C26 C25 . -1.2(7)
P1 C21 C26 C25 . 179.7(4)
C21 P1 C31 C32 . -143.3(4)
C11 P1 C31 C32 . -31.9(5)
Pd1 P1 C31 C32 . 92.8(4)
C21 P1 C31 C36 . 42.0(4)
C11 P1 C31 C36 . 153.5(4)
Pd1 P1 C31 C36 . -81.8(4)
C36 C31 C32 C33 . 1.4(8)
P1 C31 C32 C33 . -173.3(4)
C31 C32 C33 C34 . -1.7(9)
C32 C33 C34 C35 . 1.6(10)
C33 C34 C35 C36 . -1.3(9)
C34 C35 C36 C31 . 1.1(8)
C32 C31 C36 C35 . -1.1(7)
P1 C31 C36 C35 . 173.7(4)
