#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:04:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178633 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/44/4074483.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4074483
loop_
_publ_author_name
'Baumgartner, Thomas'
'Fiege, Marcel'
'Pontzen, Florian'
'Arteaga-Müller, Rocio'
_publ_section_title
;
 Redox-Active, Multinuclear (Ferrocenylethynyl)phosphanes and Their
 Palladium and Platinum Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5657
_journal_paper_doi               10.1021/om0606892
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C48 H38 Fe2 I2 P2 Pd'
_chemical_formula_sum            'C48 H38 Fe2 I2 P2 Pd'
_chemical_formula_weight         1148.62
_chemical_name_common            13
_chemical_name_systematic
; 
 Bis(diphenyl(ferrocenylethynyl)phosphane)palladium diiodide 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                107.208(13)
_cell_angle_beta                 101.176(19)
_cell_angle_gamma                102.58(2)
_cell_formula_units_Z            1
_cell_length_a                   7.601(3)
_cell_length_b                   12.040(2)
_cell_length_c                   13.0166(17)
_cell_measurement_reflns_used    4636
_cell_measurement_temperature    228(2)
_cell_volume                     1067.1(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      228(2)
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .998
_diffrn_measurement_device_type  CAD4
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4634
_diffrn_reflns_theta_full        26.96
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    2.642
_exptl_absorpt_correction_T_max  0.7780
_exptl_absorpt_correction_T_min  0.3517
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.929
_refine_diff_density_min         -1.467
_refine_diff_density_rms         .246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1400P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2159
_reflns_number_gt                3979
_reflns_number_total             4634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0606892si20060731_040753.cif
_cod_data_source_block           APdI2
_cod_original_cell_volume        1067.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074483
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pd1 Pd 0.5000 0.5000 1.0000 0.0231(2) Uani 1 2 d S
Fe1 Fe 0.34702(14) 1.04648(10) 1.24749(10) 0.0285(3) Uani 1 1 d .
I1 I 0.62018(9) 0.72144(5) 1.00418(5) 0.0432(2) Uani 1 1 d .
P1 P 0.4169(3) 0.58008(16) 1.16207(16) 0.0257(4) Uani 1 1 d .
C11 C 0.2654(11) 0.4844(7) 1.2168(7) 0.0312(16) Uani 1 1 d .
C1 C 0.2972(11) 0.6873(7) 1.1588(7) 0.0326(16) Uani 1 1 d .
C22 C 0.6428(13) 0.7663(8) 1.3610(8) 0.0411(19) Uani 1 1 d .
H22A H 0.5433 0.7997 1.3595 0.049 Uiso 1 1 calc R
C21 C 0.6288(11) 0.6607(7) 1.2766(7) 0.0301(15) Uani 1 1 d .
C26 C 0.7772(13) 0.6124(10) 1.2802(9) 0.049(2) Uani 1 1 d .
H26A H 0.7683 0.5417 1.2230 0.059 Uiso 1 1 calc R
C2 C 0.2342(11) 0.7707(7) 1.1621(7) 0.0327(16) Uani 1 1 d .
C12 C 0.0825(12) 0.4214(8) 1.1529(8) 0.0382(18) Uani 1 1 d .
H12A H 0.0407 0.4234 1.0816 0.046 Uiso 1 1 calc R
C23 C 0.8070(14) 0.8223(9) 1.4482(8) 0.047(2) Uani 1 1 d .
H23A H 0.8182 0.8944 1.5045 0.056 Uiso 1 1 calc R
C31 C 0.1704(10) 0.8743(7) 1.1694(7) 0.0307(16) Uani 1 1 d .
C33 C 0.0740(10) 1.0417(7) 1.2410(8) 0.0374(18) Uani 1 1 d .
H33A H 0.0330 1.1035 1.2905 0.045 Uiso 1 1 calc R
C32 C 0.1081(10) 0.9391(7) 1.2607(7) 0.0319(16) Uani 1 1 d .
H32A H 0.0945 0.9163 1.3257 0.038 Uiso 1 1 calc R
C34 C 0.1104(13) 1.0427(9) 1.1389(9) 0.045(2) Uani 1 1 d .
H34A H 0.0977 1.1044 1.1052 0.055 Uiso 1 1 calc R
C35 C 0.1732(12) 0.9406(8) 1.0949(8) 0.0394(18) Uani 1 1 d .
H35A H 0.2087 0.9183 1.0248 0.047 Uiso 1 1 calc R
C24 C 0.9522(13) 0.7723(10) 1.4518(8) 0.052(3) Uani 1 1 d .
H24A H 1.0602 0.8093 1.5115 0.062 Uiso 1 1 calc R
C16 C 0.3289(12) 0.4771(9) 1.3214(8) 0.041(2) Uani 1 1 d .
H16A H 0.4528 0.5166 1.3637 0.050 Uiso 1 1 calc R
C13 C -0.0388(13) 0.3550(9) 1.1959(11) 0.052(3) Uani 1 1 d .
H13A H -0.1624 0.3140 1.1537 0.063 Uiso 1 1 calc R
C36 C 0.5417(14) 1.2077(9) 1.2778(10) 0.051(2) Uani 1 1 d .
H36A H 0.5193 1.2733 1.2520 0.061 Uiso 1 1 calc R
C39 C 0.6132(12) 1.0362(10) 1.2854(11) 0.054(3) Uani 1 1 d .
H39A H 0.6495 0.9610 1.2658 0.065 Uiso 1 1 calc R
C37 C 0.5223(14) 1.1952(9) 1.3778(9) 0.051(2) Uani 1 1 d .
H37A H 0.4844 1.2507 1.4352 0.061 Uiso 1 1 calc R
C38 C 0.5675(13) 1.0876(11) 1.3830(10) 0.055(3) Uani 1 1 d .
H38A H 0.5676 1.0564 1.4446 0.066 Uiso 1 1 calc R
C14 C 0.0227(15) 0.3497(9) 1.2997(10) 0.051(3) Uani 1 1 d .
H14A H -0.0586 0.3053 1.3280 0.062 Uiso 1 1 calc R
C40 C 0.5978(13) 1.1078(11) 1.2185(11) 0.055(3) Uani 1 1 d .
H40A H 0.6229 1.0927 1.1453 0.067 Uiso 1 1 calc R
C25 C 0.9395(15) 0.6677(11) 1.3678(10) 0.057(3) Uani 1 1 d .
H25A H 1.0390 0.6343 1.3698 0.069 Uiso 1 1 calc R
C15 C 0.2051(16) 0.4103(10) 1.3621(10) 0.055(3) Uani 1 1 d .
H15A H 0.2464 0.4065 1.4327 0.066 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
P1 Pd1 P1 179.999(1) 2_667 .
P1 Pd1 I1 87.75(5) 2_667 2_667
P1 Pd1 I1 92.26(5) . 2_667
P1 Pd1 I1 92.25(5) 2_667 .
P1 Pd1 I1 87.75(5) . .
I1 Pd1 I1 179.999(1) 2_667 .
C35 Fe1 C39 118.5(4) . .
C35 Fe1 C37 161.2(4) . .
C39 Fe1 C37 67.7(5) . .
C35 Fe1 C31 41.2(4) . .
C39 Fe1 C31 108.2(4) . .
C37 Fe1 C31 157.0(4) . .
C35 Fe1 C38 154.0(4) . .
C39 Fe1 C38 39.9(5) . .
C37 Fe1 C38 41.0(5) . .
C31 Fe1 C38 121.2(4) . .
C35 Fe1 C40 104.7(5) . .
C39 Fe1 C40 40.3(5) . .
C37 Fe1 C40 67.8(5) . .
C31 Fe1 C40 124.7(4) . .
C38 Fe1 C40 67.9(5) . .
C35 Fe1 C34 40.9(4) . .
C39 Fe1 C34 152.6(5) . .
C37 Fe1 C34 125.8(4) . .
C31 Fe1 C34 68.6(3) . .
C38 Fe1 C34 164.9(5) . .
C40 Fe1 C34 117.6(5) . .
C35 Fe1 C36 123.6(4) . .
C39 Fe1 C36 67.8(4) . .
C37 Fe1 C36 39.7(5) . .
C31 Fe1 C36 161.8(4) . .
C38 Fe1 C36 67.9(5) . .
C40 Fe1 C36 40.8(5) . .
C34 Fe1 C36 106.3(4) . .
C35 Fe1 C33 68.6(4) . .
C39 Fe1 C33 165.9(5) . .
C37 Fe1 C33 109.7(4) . .
C31 Fe1 C33 68.4(3) . .
C38 Fe1 C33 129.1(5) . .
C40 Fe1 C33 153.0(4) . .
C34 Fe1 C33 40.4(4) . .
C36 Fe1 C33 119.8(4) . .
C35 Fe1 C32 69.1(4) . .
C39 Fe1 C32 128.7(4) . .
C37 Fe1 C32 122.5(4) . .
C31 Fe1 C32 41.2(3) . .
C38 Fe1 C32 111.0(4) . .
C40 Fe1 C32 164.1(4) . .
C34 Fe1 C32 67.9(4) . .
C36 Fe1 C32 154.7(4) . .
C33 Fe1 C32 39.9(3) . .
C1 P1 C21 105.0(4) . .
C1 P1 C11 99.8(4) . .
C21 P1 C11 104.7(4) . .
C1 P1 Pd1 114.5(3) . .
C21 P1 Pd1 108.7(3) . .
C11 P1 Pd1 122.3(3) . .
C16 C11 C12 119.7(8) . .
C16 C11 P1 121.5(6) . .
C12 C11 P1 118.8(7) . .
C2 C1 P1 172.6(7) . .
C21 C22 C23 119.4(9) . .
C21 C22 H22A 120.3 . .
C23 C22 H22A 120.3 . .
C26 C21 C22 119.5(8) . .
C26 C21 P1 118.5(7) . .
C22 C21 P1 121.9(6) . .
C21 C26 C25 120.9(10) . .
C21 C26 H26A 119.5 . .
C25 C26 H26A 119.5 . .
C1 C2 C31 176.6(9) . .
C11 C12 C13 119.8(9) . .
C11 C12 H12A 120.1 . .
C13 C12 H12A 120.1 . .
C24 C23 C22 120.5(9) . .
C24 C23 H23A 119.8 . .
C22 C23 H23A 119.8 . .
C2 C31 C35 126.9(8) . .
C2 C31 C32 125.5(8) . .
C35 C31 C32 107.3(7) . .
C2 C31 Fe1 121.9(5) . .
C35 C31 Fe1 68.7(5) . .
C32 C31 Fe1 70.2(4) . .
C32 C33 C34 109.0(7) . .
C32 C33 Fe1 70.4(4) . .
C34 C33 Fe1 69.6(5) . .
C32 C33 H33A 125.5 . .
C34 C33 H33A 125.5 . .
Fe1 C33 H33A 125.5 . .
C33 C32 C31 107.7(8) . .
C33 C32 Fe1 69.7(5) . .
C31 C32 Fe1 68.6(4) . .
C33 C32 H32A 126.1 . .
C31 C32 H32A 126.1 . .
Fe1 C32 H32A 126.1 . .
C33 C34 C35 108.1(8) . .
C33 C34 Fe1 70.0(5) . .
C35 C34 Fe1 68.5(5) . .
C33 C34 H34A 125.9 . .
C35 C34 H34A 125.9 . .
Fe1 C34 H34A 125.9 . .
C34 C35 C31 107.8(8) . .
C34 C35 Fe1 70.6(5) . .
C31 C35 Fe1 70.1(5) . .
C34 C35 H35A 126.1 . .
C31 C35 H35A 126.1 . .
Fe1 C35 H35A 126.1 . .
C23 C24 C25 120.4(9) . .
C23 C24 H24A 119.8 . .
C25 C24 H24A 119.8 . .
C11 C16 C15 119.2(9) . .
C11 C16 H16A 120.4 . .
C15 C16 H16A 120.4 . .
C14 C13 C12 120.4(9) . .
C14 C13 H13A 119.8 . .
C12 C13 H13A 119.8 . .
C37 C36 C40 108.1(10) . .
C37 C36 Fe1 69.8(6) . .
C40 C36 Fe1 69.3(5) . .
C37 C36 H36A 126.0 . .
C40 C36 H36A 126.0 . .
Fe1 C36 H36A 126.0 . .
C38 C39 C40 109.4(10) . .
C38 C39 Fe1 70.4(5) . .
C40 C39 Fe1 70.2(5) . .
C38 C39 H39A 125.3 . .
C40 C39 H39A 125.3 . .
Fe1 C39 H39A 125.3 . .
C36 C37 C38 108.3(10) . .
C36 C37 Fe1 70.5(6) . .
C38 C37 Fe1 69.5(5) . .
C36 C37 H37A 125.9 . .
C38 C37 H37A 125.9 . .
Fe1 C37 H37A 125.9 . .
C39 C38 C37 107.2(10) . .
C39 C38 Fe1 69.8(6) . .
C37 C38 Fe1 69.5(5) . .
C39 C38 H38A 126.4 . .
C37 C38 H38A 126.4 . .
Fe1 C38 H38A 126.4 . .
C13 C14 C15 119.8(9) . .
C13 C14 H14A 120.1 . .
C15 C14 H14A 120.1 . .
C39 C40 C36 107.0(11) . .
C39 C40 Fe1 69.5(5) . .
C36 C40 Fe1 69.9(5) . .
C39 C40 H40A 126.5 . .
C36 C40 H40A 126.5 . .
Fe1 C40 H40A 126.5 . .
C24 C25 C26 119.3(10) . .
C24 C25 H25A 120.3 . .
C26 C25 H25A 120.3 . .
C14 C15 C16 121.1(10) . .
C14 C15 H15A 119.5 . .
C16 C15 H15A 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 P1 2.3147(19) 2_667
Pd1 P1 2.3148(19) .
Pd1 I1 2.6036(7) 2_667
Pd1 I1 2.6036(7) .
Fe1 C35 2.016(9) .
Fe1 C39 2.027(9) .
Fe1 C37 2.036(10) .
Fe1 C31 2.035(8) .
Fe1 C38 2.035(9) .
Fe1 C40 2.037(9) .
Fe1 C34 2.043(9) .
Fe1 C36 2.045(9) .
Fe1 C33 2.048(8) .
Fe1 C32 2.056(8) .
P1 C1 1.739(8) .
P1 C21 1.814(8) .
P1 C11 1.839(9) .
C11 C16 1.389(12) .
C11 C12 1.385(12) .
C1 C2 1.197(11) .
C22 C21 1.380(12) .
C22 C23 1.390(13) .
C22 H22A 0.9300 .
C21 C26 1.375(12) .
C26 C25 1.383(14) .
C26 H26A 0.9300 .
C2 C31 1.419(11) .
C12 C13 1.396(13) .
C12 H12A 0.9300 .
C23 C24 1.368(16) .
C23 H23A 0.9300 .
C31 C35 1.427(12) .
C31 C32 1.440(12) .
C33 C32 1.401(12) .
C33 C34 1.412(15) .
C33 H33A 0.9800 .
C32 H32A 0.9800 .
C34 C35 1.418(13) .
C34 H34A 0.9800 .
C35 H35A 0.9800 .
C24 C25 1.371(16) .
C24 H24A 0.9300 .
C16 C15 1.389(13) .
C16 H16A 0.9300 .
C13 C14 1.366(17) .
C13 H13A 0.9300 .
C36 C37 1.386(16) .
C36 C40 1.422(16) .
C36 H36A 0.9800 .
C39 C38 1.385(17) .
C39 C40 1.401(16) .
C39 H39A 0.9800 .
C37 C38 1.427(16) .
C37 H37A 0.9800 .
C38 H38A 0.9800 .
C14 C15 1.373(16) .
C14 H14A 0.9300 .
C40 H40A 0.9800 .
C25 H25A 0.9300 .
C15 H15A 0.9300 .
