#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:31:00 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179688 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/10/7001072.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_7001072
loop_
_publ_author_name
'Koshevoy, Igor O.'
'Gutierrez-Puebla, Enrique'
'Lahuerta, Pascual'
'Monge, Angeles'
'Ubeda, M.Angeles'
'Sanaú, Mercedes'
_publ_section_title
;
 Isolation of enantiomerically pure organometallic palladium compounds:
 synthesis of the triangles prepared from enantiopure
 [cis-Pd2(C6H4PPh2)2(NCCH3)4]2+
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              2993
_journal_page_last               2998
_journal_paper_doi               10.1039/b816803b
_journal_year                    2009
_chemical_formula_sum            'C76 H68 Br4 O2 P4 Pd4'
_chemical_formula_weight         1882.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.135(3)
_cell_length_b                   22.135(3)
_cell_length_c                   15.515(3)
_cell_measurement_reflns_used    30291
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     7602(2)
_computing_cell_refinement       'Denzo & Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect(Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.2001
_diffrn_reflns_av_sigmaI/netI    0.1059
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22385
_diffrn_reflns_theta_full        22.04
_diffrn_reflns_theta_max         22.04
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    3.161
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.005
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.363
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.0050(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         4670
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1027P)²+18.7012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                4111
_reflns_number_total             4670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816803b.txt
_cod_data_source_block           SS-1
_cod_original_cell_volume        7601(2)
_cod_original_sg_symbol_H-M      P43212
_cod_database_code               7001072
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'
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
Pd1 Pd 0.66161(5) 0.74304(5) 0.08827(8) 0.0340(4) Uani 1 1 d U . .
Br1 Br 0.75066(7) 0.67498(8) 0.08702(11) 0.0471(5) Uani 1 1 d U . .
P1 P 0.58067(19) 0.8034(2) 0.1037(3) 0.0389(11) Uani 1 1 d U . .
O1 O 0.3597(11) 0.8364(12) 0.923(2) 0.216(14) Uani 1 1 d DU . .
H1A H 0.3520 0.8671 0.8954 0.324 Uiso 1 1 calc R . .
Pd2 Pd 0.57316(6) 0.63753(6) 0.10768(8) 0.0372(4) Uani 1 1 d U . .
Br2 Br 0.63731(9) 0.54477(8) 0.05935(11) 0.0483(5) Uani 1 1 d U . .
P2 P 0.5954(2) 0.6419(2) 0.2594(3) 0.0402(11) Uani 1 1 d U . .
C11 C 0.5135(8) 0.7620(8) 0.1366(12) 0.048(4) Uani 1 1 d U . .
C12 C 0.5101(7) 0.7028(8) 0.1385(11) 0.046(3) Uani 1 1 d U . .
C13 C 0.4527(8) 0.6762(9) 0.1527(12) 0.055(4) Uani 1 1 d U . .
H13A H 0.4488 0.6345 0.1488 0.065 Uiso 1 1 calc R . .
C14 C 0.4031(8) 0.7101(11) 0.1721(12) 0.066(5) Uani 1 1 d U . .
H14A H 0.3663 0.6919 0.1850 0.079 Uiso 1 1 calc R . .
C15 C 0.4088(8) 0.7686(11) 0.1720(13) 0.065(5) Uani 1 1 d U . .
H15A H 0.3749 0.7916 0.1848 0.077 Uiso 1 1 calc R . .
C16 C 0.4609(8) 0.7981(9) 0.1544(11) 0.055(4) Uani 1 1 d U . .
H16A H 0.4626 0.8401 0.1539 0.066 Uiso 1 1 calc R . .
C21 C 0.5903(5) 0.8638(4) 0.1935(6) 0.049(4) Uani 1 1 d GU . .
C22 C 0.5625(5) 0.8645(5) 0.2738(7) 0.053(4) Uani 1 1 d GU . .
H22A H 0.5341 0.8351 0.2878 0.064 Uiso 1 1 calc R . .
C23 C 0.5771(6) 0.9092(6) 0.3332(6) 0.075(6) Uani 1 1 d GU . .
H23A H 0.5585 0.9097 0.3870 0.090 Uiso 1 1 calc R . .
C24 C 0.6195(6) 0.9532(5) 0.3123(7) 0.072(5) Uani 1 1 d GU . .
H24A H 0.6292 0.9831 0.3521 0.086 Uiso 1 1 calc R . .
C25 C 0.6473(5) 0.9524(5) 0.2320(8) 0.060(4) Uani 1 1 d GU . .
H25A H 0.6756 0.9818 0.2180 0.072 Uiso 1 1 calc R . .
C26 C 0.6327(5) 0.9077(5) 0.1726(6) 0.045(3) Uani 1 1 d GU . .
H26A H 0.6513 0.9072 0.1189 0.054 Uiso 1 1 calc R . .
C31 C 0.5518(8) 0.8445(8) 0.0033(11) 0.046(4) Uani 1 1 d U . .
C32 C 0.5465(9) 0.9066(8) -0.0015(11) 0.056(4) Uani 1 1 d U . .
H32A H 0.5568 0.9315 0.0445 0.067 Uiso 1 1 calc R . .
C33 C 0.5249(11) 0.9301(10) -0.0796(12) 0.071(5) Uani 1 1 d U . .
H33A H 0.5168 0.9713 -0.0787 0.085 Uiso 1 1 calc R . .
C34 C 0.5138(11) 0.9027(11) -0.1567(13) 0.076(5) Uani 1 1 d U . .
H34A H 0.5045 0.9235 -0.2071 0.091 Uiso 1 1 calc R . .
C35 C 0.5178(8) 0.8425(10) -0.1516(12) 0.062(5) Uani 1 1 d U . .
H35A H 0.5058 0.8197 -0.1990 0.074 Uiso 1 1 calc R . .
C36 C 0.5405(9) 0.8100(10) -0.0735(12) 0.061(5) Uani 1 1 d U . .
H36A H 0.5472 0.7685 -0.0747 0.073 Uiso 1 1 calc R . .
C41 C 0.6340(4) 0.7120(5) 0.2935(6) 0.041(3) Uani 1 1 d GU . .
C42 C 0.6662(5) 0.7457(5) 0.2334(5) 0.039(3) Uani 1 1 d GU . .
C43 C 0.7058(5) 0.7905(5) 0.2609(7) 0.049(4) Uani 1 1 d GU . .
H43A H 0.7273 0.8131 0.2207 0.059 Uiso 1 1 calc R . .
C44 C 0.7132(5) 0.8015(5) 0.3485(7) 0.064(5) Uani 1 1 d GU . .
H44A H 0.7397 0.8315 0.3669 0.077 Uiso 1 1 calc R . .
C45 C 0.6810(6) 0.7678(6) 0.4085(5) 0.069(5) Uani 1 1 d GU . .
H45A H 0.6860 0.7752 0.4671 0.083 Uiso 1 1 calc R . .
C46 C 0.6415(5) 0.7230(5) 0.3810(5) 0.056(4) Uani 1 1 d GU . .
H46A H 0.6200 0.7005 0.4212 0.067 Uiso 1 1 calc R . .
C50 C 0.3810(14) 0.7285(17) 0.892(3) 0.206(19) Uani 1 1 d U . .
H50A H 0.3907 0.7024 0.8447 0.309 Uiso 1 1 calc R . .
H50B H 0.3449 0.7145 0.9199 0.309 Uiso 1 1 calc R . .
H50C H 0.4137 0.7284 0.9328 0.309 Uiso 1 1 calc R . .
C51 C 0.5326(8) 0.6375(9) 0.3400(11) 0.051(4) Uani 1 1 d U . .
C52 C 0.5192(11) 0.5832(11) 0.3903(13) 0.084(6) Uani 1 1 d U . .
H52A H 0.5413 0.5479 0.3826 0.101 Uiso 1 1 calc R . .
C53 C 0.4717(11) 0.5861(12) 0.4507(15) 0.086(6) Uani 1 1 d U . .
H53A H 0.4640 0.5520 0.4840 0.104 Uiso 1 1 calc R . .
C54 C 0.4373(10) 0.6347(13) 0.4628(13) 0.080(5) Uani 1 1 d U . .
H54A H 0.4051 0.6340 0.5013 0.096 Uiso 1 1 calc R . .
C55 C 0.4502(9) 0.6844(12) 0.4182(13) 0.072(5) Uani 1 1 d U . .
H55A H 0.4271 0.7188 0.4280 0.087 Uiso 1 1 calc R . .
C56 C 0.4973(9) 0.6877(11) 0.3566(13) 0.068(5) Uani 1 1 d U . .
H56A H 0.5045 0.7237 0.3273 0.082 Uiso 1 1 calc R . .
C60 C 0.3722(15) 0.7860(19) 0.862(3) 0.222(18) Uani 1 1 d DU . .
H60A H 0.3388 0.7844 0.8220 0.267 Uiso 1 1 calc R . .
H60B H 0.4078 0.7970 0.8296 0.267 Uiso 1 1 calc R . .
C61 C 0.6454(8) 0.5800(8) 0.2956(10) 0.047(3) Uani 1 1 d U . .
C62 C 0.6976(9) 0.5912(9) 0.3371(13) 0.063(5) Uani 1 1 d U . .
H62A H 0.7094 0.6309 0.3480 0.075 Uiso 1 1 calc R . .
C63 C 0.7347(11) 0.5429(11) 0.3640(15) 0.084(6) Uani 1 1 d U . .
H63A H 0.7701 0.5508 0.3942 0.100 Uiso 1 1 calc R . .
C64 C 0.7186(13) 0.4838(11) 0.3459(14) 0.089(6) Uani 1 1 d U . .
H64A H 0.7420 0.4514 0.3647 0.106 Uiso 1 1 calc R . .
C65 C 0.6645(12) 0.4745(10) 0.2971(13) 0.076(5) Uani 1 1 d U . .
H65A H 0.6542 0.4359 0.2785 0.091 Uiso 1 1 calc R . .
C66 C 0.6276(10) 0.5229(9) 0.2778(13) 0.063(5) Uani 1 1 d U . .
H66A H 0.5902 0.5162 0.2523 0.076 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
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'
O O 0.0106 0.0060 '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'
Br Br -0.2901 2.4595 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Pd1 C42 85.0(3) . . ?
P1 Pd1 Br1 174.28(13) . . ?
C42 Pd1 Br1 89.3(3) . . ?
P1 Pd1 Br1 98.94(13) . 7 ?
C42 Pd1 Br1 169.9(3) . 7 ?
Br1 Pd1 Br1 86.78(7) . 7 ?
P1 Pd1 Pd2 86.17(12) . . ?
C42 Pd1 Pd2 87.2(3) . . ?
Br1 Pd1 Pd2 92.61(6) . . ?
Br1 Pd1 Pd2 102.33(6) 7 . ?
Pd1 Br1 Pd1 91.40(6) . 7 ?
C11 P1 C31 101.2(8) . . ?
C11 P1 C21 103.6(7) . . ?
C31 P1 C21 107.0(7) . . ?
C11 P1 Pd1 112.5(6) . . ?
C31 P1 Pd1 117.5(5) . . ?
C21 P1 Pd1 113.4(4) . . ?
C12 Pd2 P2 83.3(5) . . ?
C12 Pd2 Br2 170.4(5) . . ?
P2 Pd2 Br2 101.61(12) . . ?
C12 Pd2 Br2 93.8(5) . 7 ?
P2 Pd2 Br2 177.17(13) . 7 ?
Br2 Pd2 Br2 81.22(7) . 7 ?
C12 Pd2 Pd1 85.5(5) . . ?
P2 Pd2 Pd1 86.26(11) . . ?
Br2 Pd2 Pd1 102.95(6) . . ?
Br2 Pd2 Pd1 93.24(6) 7 . ?
Pd2 Br2 Pd2 95.45(7) . 7 ?
C61 P2 C41 105.0(7) . . ?
C61 P2 C51 101.7(8) . . ?
C41 P2 C51 101.3(7) . . ?
C61 P2 Pd2 113.0(6) . . ?
C41 P2 Pd2 114.1(4) . . ?
C51 P2 Pd2 119.9(6) . . ?
C12 C11 C16 120.2(17) . . ?
C12 C11 P1 123.7(14) . . ?
C16 C11 P1 115.9(14) . . ?
C11 C12 C13 118.0(17) . . ?
C11 C12 Pd2 130.8(14) . . ?
C13 C12 Pd2 110.6(13) . . ?
C14 C13 C12 121.8(19) . . ?
C15 C14 C13 118.0(19) . . ?
C14 C15 C16 124.3(19) . . ?
C15 C16 C11 117.4(18) . . ?
C22 C21 C26 120.0 . . ?
C22 C21 P1 127.0(6) . . ?
C26 C21 P1 112.9(6) . . ?
C23 C22 C21 120.0 . . ?
C24 C23 C22 120.0 . . ?
C23 C24 C25 120.0 . . ?
C24 C25 C26 120.0 . . ?
C25 C26 C21 120.0 . . ?
C32 C31 C36 117.9(17) . . ?
C32 C31 P1 123.1(15) . . ?
C36 C31 P1 118.7(13) . . ?
C31 C32 C33 116.4(19) . . ?
C34 C33 C32 131(2) . . ?
C35 C34 C33 112.3(19) . . ?
C34 C35 C36 123.3(19) . . ?
C31 C36 C35 118.3(18) . . ?
C42 C41 C46 120.0 . . ?
C42 C41 P2 119.8(6) . . ?
C46 C41 P2 118.8(6) . . ?
C41 C42 C43 120.0 . . ?
C41 C42 Pd1 129.2(5) . . ?
C43 C42 Pd1 110.7(5) . . ?
C44 C43 C42 120.0 . . ?
C43 C44 C45 120.0 . . ?
C44 C45 C46 120.0 . . ?
C45 C46 C41 120.0 . . ?
C56 C51 C52 116.5(18) . . ?
C56 C51 P2 120.2(15) . . ?
C52 C51 P2 123.2(16) . . ?
C53 C52 C51 118(2) . . ?
C54 C53 C52 124(2) . . ?
C55 C54 C53 118(2) . . ?
C54 C55 C56 124(2) . . ?
C51 C56 C55 120(2) . . ?
C50 C60 O1 121(4) . . ?
C62 C61 C66 121.2(19) . . ?
C62 C61 P2 121.5(15) . . ?
C66 C61 P2 117.2(14) . . ?
C61 C62 C63 120(2) . . ?
C64 C63 C62 120(2) . . ?
C63 C64 C65 117(2) . . ?
C66 C65 C64 120(2) . . ?
C61 C66 C65 121(2) . . ?
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
Pd1 P1 2.247(4) . ?
Pd1 C42 2.255(7) . ?
Pd1 Br1 2.481(2) . ?
Pd1 Br1 2.741(2) 7 ?
Pd1 Pd2 3.0625(18) . ?
Br1 Pd1 2.741(2) 7 ?
P1 C11 1.820(18) . ?
P1 C31 1.914(17) . ?
P1 C21 1.942(9) . ?
O1 C60 1.484(19) . ?
Pd2 C12 2.065(17) . ?
Pd2 P2 2.407(4) . ?
Pd2 Br2 2.607(2) . ?
Pd2 Br2 2.667(2) 7 ?
Br2 Pd2 2.667(2) 7 ?
P2 C61 1.846(18) . ?
P2 C41 1.848(9) . ?
P2 C51 1.872(17) . ?
C11 C12 1.31(2) . ?
C11 C16 1.44(2) . ?
C12 C13 1.42(2) . ?
C13 C14 1.36(3) . ?
C14 C15 1.30(3) . ?
C15 C16 1.35(3) . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C31 C32 1.38(2) . ?
C31 C36 1.44(3) . ?
C32 C33 1.40(3) . ?
C33 C34 1.36(3) . ?
C34 C35 1.34(3) . ?
C35 C36 1.50(2) . ?
C41 C42 1.3900 . ?
C41 C46 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C44 C45 1.3900 . ?
C45 C46 1.3900 . ?
C50 C60 1.37(5) . ?
C51 C56 1.38(3) . ?
C51 C52 1.46(3) . ?
C52 C53 1.41(3) . ?
C53 C54 1.33(3) . ?
C54 C55 1.33(3) . ?
C55 C56 1.42(3) . ?
C61 C62 1.35(2) . ?
C61 C66 1.35(3) . ?
C62 C63 1.41(3) . ?
C63 C64 1.39(3) . ?
C64 C65 1.43(3) . ?
C65 C66 1.38(3) . ?
