#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/70/2237086.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_2237086
loop_
_publ_author_name
'Brown, Shayne'
'Crundwell, Guy'
_publ_section_title
;
 Di-μ-iodido-bis[(biphenyl-2-yl)(triphenylphosphane-κP)palladium(II)]
;
_journal_coeditor_code           YK2076
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1526
_journal_paper_doi               10.1107/S1600536812047733
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd2 (C12 H9)2 I2 (C18 H15 P)2]'
_chemical_formula_moiety         'C60 H48 I2 P2 Pd2'
_chemical_formula_sum            'C60 H48 I2 P2 Pd2'
_chemical_formula_weight         1297.52
_chemical_melting_point          423
_chemical_name_systematic
;
Di-μ-iodido-bis[(biphenyl-2-yl)(triphenylphosphane-κP)palladium(II)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 133.962(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6957(4)
_cell_length_b                   20.0969(10)
_cell_length_c                   18.3718(7)
_cell_measurement_reflns_used    4701
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5692
_cell_measurement_theta_min      4.1238
_cell_volume                     2576.7(3)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1790
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12030
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         4.26
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.924
_refine_diff_density_min         -0.768
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0678P)²+0.4388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                3783
_reflns_number_total             6087
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            yk2076.cif
_cod_data_source_block           I
_cod_original_cell_volume        2576.8(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2237086
_cod_database_fobs_code          2237086
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
Pd Pd1 0.79025(6) 0.05054(2) 0.37739(3) 0.04167(15) Uani d . 1 1
I I1 1.16659(5) 0.06784(2) 0.53368(3) 0.05752(17) Uani d . 1 1
C C1 0.7754(8) 0.1416(4) 0.3248(4) 0.0551(17) Uani d . 1 1
C C2 0.8449(9) 0.1495(4) 0.2822(5) 0.067(2) Uani d . 1 1
H H2 0.9040 0.1142 0.2801 0.081 Uiso calc R 1 1
C C3 0.8265(13) 0.2129(6) 0.2404(6) 0.088(3) Uani d . 1 1
H H3 0.8758 0.2197 0.2121 0.106 Uiso calc R 1 1
C C4 0.7348(15) 0.2634(5) 0.2430(7) 0.100(3) Uani d . 1 1
H H4 0.7177 0.3040 0.2135 0.120 Uiso calc R 1 1
C C5 0.6681(12) 0.2555(4) 0.2877(6) 0.083(3) Uani d . 1 1
H H5 0.6088 0.2910 0.2895 0.099 Uiso calc R 1 1
C C6 0.6881(9) 0.1952(3) 0.3305(5) 0.0588(18) Uani d . 1 1
C C7 0.6180(11) 0.1889(4) 0.3831(6) 0.068(2) Uani d . 1 1
C C8 0.7372(13) 0.1662(4) 0.4818(6) 0.079(2) Uani d . 1 1
H H8 0.8631 0.1549 0.5171 0.095 Uiso calc R 1 1
C C9 0.6734(18) 0.1603(5) 0.5279(8) 0.106(3) Uani d . 1 1
H H9 0.7567 0.1455 0.5944 0.127 Uiso calc R 1 1
C C10 0.489(2) 0.1758(6) 0.4780(12) 0.119(4) Uani d . 1 1
H H10 0.4438 0.1685 0.5086 0.143 Uiso calc R 1 1
C C11 0.3707(18) 0.2021(6) 0.3832(11) 0.112(4) Uani d . 1 1
H H11 0.2478 0.2155 0.3512 0.134 Uiso calc R 1 1
C C12 0.4308(12) 0.2092(5) 0.3339(8) 0.092(3) Uani d . 1 1
H H12 0.3492 0.2272 0.2691 0.110 Uiso calc R 1 1
P P3 0.4805(2) 0.03204(8) 0.23017(10) 0.0410(4) Uani d . 1 1
C C13 0.4662(8) -0.0292(3) 0.1506(4) 0.0480(15) Uani d . 1 1
C C14 0.6076(11) -0.0734(4) 0.1914(6) 0.071(2) Uani d . 1 1
H H14 0.7146 -0.0723 0.2607 0.085 Uiso calc R 1 1
C C15 0.5987(12) -0.1206(4) 0.1328(7) 0.086(3) Uani d . 1 1
H H15 0.6977 -0.1510 0.1627 0.103 Uiso calc R 1 1
C C16 0.4449(14) -0.1217(5) 0.0326(7) 0.086(3) Uani d . 1 1
H H16 0.4369 -0.1535 -0.0071 0.104 Uiso calc R 1 1
C C17 0.3022(14) -0.0773(5) -0.0111(6) 0.093(3) Uani d . 1 1
H H17 0.1976 -0.0781 -0.0808 0.112 Uiso calc R 1 1
C C18 0.3103(11) -0.0303(4) 0.0472(5) 0.080(2) Uani d . 1 1
H H18 0.2114 0.0002 0.0168 0.097 Uiso calc R 1 1
C C19 0.3357(8) -0.0016(3) 0.2508(4) 0.0459(14) Uani d . 1 1
C C20 0.1854(10) -0.0459(4) 0.1846(5) 0.0637(19) Uani d . 1 1
H H20 0.1653 -0.0646 0.1315 0.076 Uiso calc R 1 1
C C21 0.0680(11) -0.0617(4) 0.1982(7) 0.080(2) Uani d . 1 1
H H21 -0.0323 -0.0914 0.1542 0.096 Uiso calc R 1 1
C C22 0.0958(12) -0.0342(5) 0.2767(7) 0.087(3) Uani d . 1 1
H H22 0.0118 -0.0442 0.2836 0.105 Uiso calc R 1 1
C C23 0.2466(12) 0.0077(5) 0.3437(7) 0.079(2) Uani d . 1 1
H H23 0.2669 0.0255 0.3973 0.095 Uiso calc R 1 1
C C24 0.3684(9) 0.0237(4) 0.3323(5) 0.0603(18) Uani d . 1 1
H H24 0.4727 0.0514 0.3789 0.072 Uiso calc R 1 1
C C25 0.3342(8) 0.1009(3) 0.1431(4) 0.0488(15) Uani d . 1 1
C C26 0.1787(10) 0.1252(4) 0.1242(6) 0.075(2) Uani d . 1 1
H H26 0.1425 0.1057 0.1548 0.090 Uiso calc R 1 1
C C27 0.0765(12) 0.1788(5) 0.0592(7) 0.097(3) Uani d . 1 1
H H27 -0.0303 0.1947 0.0449 0.116 Uiso calc R 1 1
C C28 0.1319(12) 0.2082(5) 0.0165(7) 0.089(3) Uani d . 1 1
H H28 0.0675 0.2458 -0.0234 0.107 Uiso calc R 1 1
C C29 0.2765(12) 0.1840(4) 0.0309(6) 0.080(2) Uani d . 1 1
H H29 0.3082 0.2032 -0.0019 0.097 Uiso calc R 1 1
C C30 0.3794(10) 0.1307(4) 0.0942(5) 0.068(2) Uani d . 1 1
H H30 0.4813 0.1143 0.1042 0.082 Uiso calc R 1 1
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'
I I -0.4742 1.8119 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Pd1 P3 . 89.00(16) no
C1 Pd1 I1 . 89.25(16) no
P3 Pd1 I1 . 171.22(4) no
C1 Pd1 I1 3_756 174.70(18) no
P3 Pd1 I1 3_756 95.49(4) no
I1 Pd1 I1 3_756 86.730(18) no
Pd1 I1 Pd1 3_756 93.270(18) no
C2 C1 C6 . 121.2(7) no
C2 C1 Pd1 . 118.9(6) no
C6 C1 Pd1 . 119.9(5) no
C1 C2 C3 . 119.2(8) no
C1 C2 H2 . 120.4 no
C3 C2 H2 . 120.4 no
C4 C3 C2 . 118.7(8) no
C4 C3 H3 . 120.6 no
C2 C3 H3 . 120.6 no
C5 C4 C3 . 121.8(9) no
C5 C4 H4 . 119.1 no
C3 C4 H4 . 119.1 no
C4 C5 C6 . 120.4(9) no
C4 C5 H5 . 119.8 no
C6 C5 H5 . 119.8 no
C5 C6 C1 . 118.6(7) no
C5 C6 C7 . 119.0(7) no
C1 C6 C7 . 122.4(6) no
C8 C7 C12 . 117.8(8) no
C8 C7 C6 . 121.5(7) no
C12 C7 C6 . 120.6(8) no
C9 C8 C7 . 121.2(9) no
C9 C8 H8 . 119.4 no
C7 C8 H8 . 119.4 no
C8 C9 C10 . 121.0(11) no
C8 C9 H9 . 119.5 no
C10 C9 H9 . 119.5 no
C11 C10 C9 . 119.5(12) no
C11 C10 H10 . 120.3 no
C9 C10 H10 . 120.3 no
C10 C11 C12 . 121.1(11) no
C10 C11 H11 . 119.5 no
C12 C11 H11 . 119.5 no
C11 C12 C7 . 119.2(10) no
C11 C12 H12 . 120.4 no
C7 C12 H12 . 120.4 no
C19 P3 C25 . 102.8(3) no
C19 P3 C13 . 105.9(3) no
C25 P3 C13 . 103.1(3) no
C19 P3 Pd1 . 112.63(19) no
C25 P3 Pd1 . 119.9(2) no
C13 P3 Pd1 . 111.23(19) no
C14 C13 C18 . 118.5(7) no
C14 C13 P3 . 120.9(5) no
C18 C13 P3 . 120.6(5) no
C13 C14 C15 . 121.9(8) no
C13 C14 H14 . 119.1 no
C15 C14 H14 . 119.1 no
C16 C15 C14 . 119.1(8) no
C16 C15 H15 . 120.5 no
C14 C15 H15 . 120.5 no
C15 C16 C17 . 120.6(8) no
C15 C16 H16 . 119.7 no
C17 C16 H16 . 119.7 no
C16 C17 C18 . 120.4(8) no
C16 C17 H17 . 119.8 no
C18 C17 H17 . 119.8 no
C13 C18 C17 . 119.6(7) no
C13 C18 H18 . 120.2 no
C17 C18 H18 . 120.2 no
C20 C19 C24 . 119.5(6) no
C20 C19 P3 . 123.1(5) no
C24 C19 P3 . 117.1(5) no
C21 C20 C19 . 119.3(7) no
C21 C20 H20 . 120.3 no
C19 C20 H20 . 120.3 no
C20 C21 C22 . 121.0(7) no
C20 C21 H21 . 119.5 no
C22 C21 H21 . 119.5 no
C23 C22 C21 . 119.9(8) no
C23 C22 H22 . 120.1 no
C21 C22 H22 . 120.1 no
C22 C23 C24 . 120.1(8) no
C22 C23 H23 . 120.0 no
C24 C23 H23 . 120.0 no
C23 C24 C19 . 120.1(7) no
C23 C24 H24 . 120.0 no
C19 C24 H24 . 120.0 no
C26 C25 C30 . 118.0(6) no
C26 C25 P3 . 122.5(5) no
C30 C25 P3 . 119.6(5) no
C25 C26 C27 . 119.5(8) no
C25 C26 H26 . 120.2 no
C27 C26 H26 . 120.2 no
C28 C27 C26 . 120.2(8) no
C28 C27 H27 . 119.9 no
C26 C27 H27 . 119.9 no
C29 C28 C27 . 121.0(8) no
C29 C28 H28 . 119.5 no
C27 C28 H28 . 119.5 no
C28 C29 C30 . 120.1(8) no
C28 C29 H29 . 119.9 no
C30 C29 H29 . 119.9 no
C29 C30 C25 . 121.1(7) no
C29 C30 H30 . 119.5 no
C25 C30 H30 . 119.5 no
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 C1 . 2.028(7) no
Pd1 P3 . 2.2792(14) no
Pd1 I1 . 2.6709(6) no
Pd1 I1 3_756 2.7486(7) no
I1 Pd1 3_756 2.7486(7) no
C1 C2 . 1.349(9) no
C1 C6 . 1.417(10) no
C2 C3 . 1.434(12) no
C2 H2 . 0.9300 no
C3 C4 . 1.372(13) no
C3 H3 . 0.9300 no
C4 C5 . 1.361(12) no
C4 H4 . 0.9300 no
C5 C6 . 1.385(10) no
C5 H5 . 0.9300 no
C6 C7 . 1.525(10) no
C7 C8 . 1.386(11) no
C7 C12 . 1.414(10) no
C8 C9 . 1.356(11) no
C8 H8 . 0.9300 no
C9 C10 . 1.366(14) no
C9 H9 . 0.9300 no
C10 C11 . 1.362(15) no
C10 H10 . 0.9300 no
C11 C12 . 1.385(13) no
C11 H11 . 0.9300 no
C12 H12 . 0.9300 no
P3 C19 . 1.821(6) no
P3 C25 . 1.827(6) no
P3 C13 . 1.842(6) no
C13 C14 . 1.342(9) no
C13 C18 . 1.381(9) no
C14 C15 . 1.392(10) no
C14 H14 . 0.9300 no
C15 C16 . 1.343(11) no
C15 H15 . 0.9300 no
C16 C17 . 1.347(12) no
C16 H16 . 0.9300 no
C17 C18 . 1.389(11) no
C17 H17 . 0.9300 no
C18 H18 . 0.9300 no
C19 C20 . 1.391(9) no
C19 C24 . 1.392(8) no
C20 C21 . 1.362(10) no
C20 H20 . 0.9300 no
C21 C22 . 1.384(12) no
C21 H21 . 0.9300 no
C22 C23 . 1.366(12) no
C22 H22 . 0.9300 no
C23 C24 . 1.374(9) no
C23 H23 . 0.9300 no
C24 H24 . 0.9300 no
C25 C26 . 1.380(9) no
C25 C30 . 1.380(9) no
C26 C27 . 1.389(11) no
C26 H26 . 0.9300 no
C27 C28 . 1.354(11) no
C27 H27 . 0.9300 no
C28 C29 . 1.326(11) no
C28 H28 . 0.9300 no
C29 C30 . 1.373(10) no
C29 H29 . 0.9300 no
C30 H30 . 0.9300 no
