#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:26:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179896 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/92/7019294.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_7019294
loop_
_publ_author_name
'Meduri, Angelo'
'Cozzula, Daniela'
'D'Amora, Angela'
'Zangrando, Ennio'
'Gladiali, Serafino'
'Milani, Barbara'
_publ_section_title
;
 Unique syndio-selectivity in CO/styrene copolymerization reaction
 catalyzed by palladium complexes with
 2-(2'-oxazolinyl)-1,10-phenanthrolines.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7474
_journal_page_last               7484
_journal_paper_doi               10.1039/c2dt30157a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C46 H40 N6 O2 Pd2 2+, 2(P F6 1-), C H2 Cl2'
_chemical_formula_sum            'C47 H42 Cl2 F12 N6 O2 P2 Pd2'
_chemical_formula_weight         1296.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           178
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61 2 (0 0 5)'
_symmetry_space_group_name_H-M   'P 61 2 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                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.1900(11)
_cell_length_b                   14.1900(11)
_cell_length_c                   42.200(4)
_cell_measurement_temperature    100(2)
_cell_volume                     7358.8(11)
_computing_data_reduction        'CCP4 Suite, 1994'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.80.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'PILATUS 2M detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.00000
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            82509
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    3.127
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3876
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_coef       0.00328(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         2120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0284
_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)+(0.0485P)²+5.6616P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                2113
_reflns_number_total             2120
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2dt30157a.txt
_cod_data_source_block           3b
_cod_original_cell_volume        7358.8(10)
_cod_database_code               7019294
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, -x, -z+5/6'
'y, x, -z+1/3'
'x-y, -y, -z'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'
'-x, -x+y, -z+2/3'
'-y, x-y, z+1/3'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'-x+y, -x, z+2/3'
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
Pd Pd 0.66625(3) 0.56669(3) 0.195071(8) 0.0242(3) Uani 1 1 d .
N1 N 0.6035(3) 0.6644(3) 0.21534(9) 0.0219(10) Uani 1 1 d .
N2 N 0.5354(3) 0.4502(3) 0.21894(10) 0.0295(11) Uani 1 1 d .
C1 C 0.6360(4) 0.7703(5) 0.21356(12) 0.0279(14) Uani 1 1 d .
C2 C 0.6008(5) 0.8230(5) 0.23439(13) 0.0388(16) Uani 1 1 d .
H2 H 0.6303 0.8995 0.2332 0.047 Uiso 1 1 calc R
C3 C 0.5235(5) 0.7631(5) 0.25658(14) 0.0438(16) Uani 1 1 d .
H3 H 0.4984 0.7973 0.2710 0.053 Uiso 1 1 calc R
C4 C 0.4817(5) 0.6504(5) 0.25774(12) 0.0354(16) Uani 1 1 d .
C5 C 0.5247(4) 0.6052(4) 0.23730(11) 0.0238(14) Uani 1 1 d .
C6 C 0.4866(4) 0.4893(4) 0.23870(12) 0.0279(14) Uani 1 1 d .
C7 C 0.4024(4) 0.4244(5) 0.25923(13) 0.0383(16) Uani 1 1 d .
C8 C 0.3619(5) 0.3114(5) 0.25813(16) 0.0518(18) Uani 1 1 d .
H8 H 0.3024 0.2632 0.2711 0.062 Uiso 1 1 calc R
C9 C 0.4094(6) 0.2726(5) 0.23829(15) 0.0510(18) Uani 1 1 d .
H9 H 0.3825 0.1964 0.2373 0.061 Uiso 1 1 calc R
C10 C 0.4970(5) 0.3423(5) 0.21930(14) 0.0388(15) Uani 1 1 d .
H10 H 0.5305 0.3129 0.2062 0.047 Uiso 1 1 calc R
C11 C 0.3976(5) 0.5796(6) 0.27947(14) 0.0555(19) Uani 1 1 d .
H11 H 0.3693 0.6102 0.2940 0.067 Uiso 1 1 calc R
C12 C 0.3585(5) 0.4730(6) 0.27978(15) 0.0483(17) Uani 1 1 d .
H12 H 0.3008 0.4285 0.2938 0.058 Uiso 1 1 calc R
C23 C 0.7109(5) 0.4583(4) 0.17914(13) 0.0368(15) Uani 1 1 d .
H23A H 0.7809 0.4976 0.1681 0.055 Uiso 1 1 calc R
H23B H 0.6554 0.4066 0.1645 0.055 Uiso 1 1 calc R
H23C H 0.7179 0.4186 0.1972 0.055 Uiso 1 1 calc R
N3 N 0.6858(3) 0.8066(3) 0.15742(9) 0.0230(10) Uani 1 1 d .
O1 O 0.7833(3) 0.9340(3) 0.19385(8) 0.0353(10) Uani 1 1 d .
C13 C 0.7035(4) 0.8343(4) 0.18680(13) 0.0266(14) Uani 1 1 d .
C14 C 0.8336(5) 0.9871(4) 0.16385(12) 0.0329(14) Uani 1 1 d .
H14 H 0.9076 0.9951 0.1627 0.039 Uiso 1 1 calc R
C15 C 0.7609(5) 0.9048(4) 0.13808(12) 0.0347(14) Uani 1 1 d .
H15 H 0.8067 0.8867 0.1242 0.042 Uiso 1 1 calc R
C16 C 0.6955(6) 0.9402(5) 0.11750(14) 0.0541(19) Uani 1 1 d .
H16A H 0.6484 0.8808 0.1031 0.081 Uiso 1 1 calc R
H16B H 0.7454 1.0043 0.1051 0.081 Uiso 1 1 calc R
H16C H 0.6506 0.9582 0.1311 0.081 Uiso 1 1 calc R
C17 C 0.8464(5) 1.0991(4) 0.16406(12) 0.0323(14) Uani 1 1 d .
C18 C 0.9404(5) 1.1856(5) 0.15068(12) 0.0379(15) Uani 1 1 d .
H18 H 0.9935 1.1723 0.1413 0.045 Uiso 1 1 calc R
C19 C 0.9566(5) 1.2906(5) 0.15096(13) 0.0396(15) Uani 1 1 d .
H19 H 1.0206 1.3488 0.1419 0.048 Uiso 1 1 calc R
C20 C 0.8800(5) 1.3094(5) 0.16428(14) 0.0415(17) Uani 1 1 d .
H20 H 0.8915 1.3814 0.1645 0.050 Uiso 1 1 calc R
C21 C 0.7860(5) 1.2261(5) 0.17737(13) 0.0381(15) Uani 1 1 d .
H21 H 0.7328 1.2399 0.1864 0.046 Uiso 1 1 calc R
C22 C 0.7711(5) 1.1214(4) 0.17702(12) 0.0344(15) Uani 1 1 d .
H22 H 0.7068 1.0636 0.1860 0.041 Uiso 1 1 calc R
P1 P 0.03529(9) 0.07059(18) 0.2500 0.0391(6) Uani 1 2 d S
F1 F 0.0319(3) 0.0690(3) 0.21217(7) 0.0577(10) Uani 1 1 d .
F2 F -0.0752(3) 0.0733(3) 0.25109(8) 0.0559(9) Uani 1 1 d .
F3 F -0.02866(19) -0.0573(4) 0.2500 0.0679(17) Uani 1 2 d S
F4 F 0.10089(19) 0.2018(4) 0.2500 0.0659(15) Uani 1 2 d S
P2 P 0.53313(9) 0.06625(18) 0.2500 0.0367(6) Uani 1 2 d S
F5 F 0.4198(2) 0.0648(2) 0.25209(8) 0.0466(9) Uani 1 1 d .
F6 F 0.5719(4) 0.1530(4) 0.22343(13) 0.126(2) Uani 1 1 d .
F7 F 0.4836(3) -0.0276(4) 0.22414(10) 0.0887(15) Uani 1 1 d .
Cl1 Cl 0.26317(16) 0.36561(16) 0.18329(4) 0.0699(6) Uani 1 1 d .
C24 C 0.2450(7) 0.2450(7) 0.1667 0.074(3) Uani 1 2 d S
H24A H 0.1881 0.2198 0.1501 0.089 Uiso 0.50 1 calc PR
H24B H 0.2198 0.1881 0.1832 0.089 Uiso 0.50 1 calc PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0074 0.0035 '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'
N N 0.0135 0.0071 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0225 0.0128 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.3471 1.8595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1741 0.1882 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0348 0.0215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
N3 Pd N2 173.45(16) 4 .
N3 Pd C23 87.2(2) 4 .
N2 Pd C23 93.0(2) . .
N3 Pd N1 99.85(16) 4 .
N2 Pd N1 79.84(17) . .
C23 Pd N1 172.78(19) . .
C1 N1 C5 116.4(4) . .
C1 N1 Pd 132.6(3) . .
C5 N1 Pd 110.3(3) . .
C10 N2 C6 117.2(5) . .
C10 N2 Pd 128.1(4) . .
C6 N2 Pd 114.5(3) . .
N1 C1 C2 123.5(5) . .
N1 C1 C13 119.4(4) . .
C2 C1 C13 116.8(5) . .
C3 C2 C1 119.2(5) . .
C2 C3 C4 118.9(5) . .
C5 C4 C3 118.3(5) . .
C5 C4 C11 118.4(5) . .
C3 C4 C11 123.3(5) . .
N1 C5 C4 123.4(5) . .
N1 C5 C6 116.7(5) . .
C4 C5 C6 119.9(5) . .
N2 C6 C7 123.7(5) . .
N2 C6 C5 117.2(5) . .
C7 C6 C5 119.1(5) . .
C6 C7 C8 117.4(6) . .
C6 C7 C12 119.8(5) . .
C8 C7 C12 122.8(6) . .
C9 C8 C7 118.8(6) . .
C8 C9 C10 121.1(6) . .
N2 C10 C9 121.7(5) . .
C12 C11 C4 122.0(6) . .
C11 C12 C7 120.6(6) . .
C13 N3 C15 107.5(4) . .
C13 N3 Pd 128.6(4) . 4
C15 N3 Pd 123.4(3) . 4
C13 O1 C14 106.9(4) . .
N3 C13 O1 118.2(5) . .
N3 C13 C1 125.8(5) . .
O1 C13 C1 115.6(5) . .
O1 C14 C17 108.0(4) . .
O1 C14 C15 104.4(4) . .
C17 C14 C15 118.9(5) . .
N3 C15 C16 110.4(5) . .
N3 C15 C14 102.4(4) . .
C16 C15 C14 115.8(5) . .
C22 C17 C18 117.9(5) . .
C22 C17 C14 123.3(5) . .
C18 C17 C14 118.8(5) . .
C19 C18 C17 120.7(5) . .
C20 C19 C18 119.5(5) . .
C19 C20 C21 121.4(5) . .
C20 C21 C22 118.4(6) . .
C17 C22 C21 122.1(5) . .
F3 P1 F2 91.22(15) . .
F3 P1 F2 91.22(15) . 6
F2 P1 F2 177.6(3) . 6
F3 P1 F1 89.29(16) . .
F2 P1 F1 90.33(18) . .
F2 P1 F1 89.70(18) 6 .
F3 P1 F1 89.29(16) . 6
F2 P1 F1 89.70(18) . 6
F2 P1 F1 90.33(18) 6 6
F1 P1 F1 178.6(3) . 6
F3 P1 F4 180.000(1) . .
F2 P1 F4 88.78(15) . .
F2 P1 F4 88.78(15) 6 .
F1 P1 F4 90.71(16) . .
F1 P1 F4 90.71(16) 6 .
F6 P2 F6 93.0(5) . 6_655
F6 P2 F7 90.1(3) . .
F6 P2 F7 176.8(4) 6_655 .
F6 P2 F7 176.8(4) . 6_655
F6 P2 F7 90.1(3) 6_655 6_655
F7 P2 F7 86.9(4) . 6_655
F6 P2 F5 90.6(2) . 6_655
F6 P2 F5 90.29(19) 6_655 6_655
F7 P2 F5 88.69(18) . 6_655
F7 P2 F5 90.4(2) 6_655 6_655
F6 P2 F5 90.29(19) . .
F6 P2 F5 90.6(2) 6_655 .
F7 P2 F5 90.4(2) . .
F7 P2 F5 88.69(18) 6_655 .
F5 P2 F5 178.8(3) 6_655 .
Cl1 C24 Cl1 111.3(5) . 4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd N3 2.027(4) 4
Pd N2 2.032(4) .
Pd C23 2.049(5) .
Pd N1 2.164(4) .
N1 C1 1.336(6) .
N1 C5 1.369(6) .
N2 C10 1.344(7) .
N2 C6 1.366(7) .
C1 C2 1.398(8) .
C1 C13 1.465(8) .
C2 C3 1.368(8) .
C3 C4 1.401(8) .
C4 C5 1.385(7) .
C4 C11 1.441(8) .
C5 C6 1.453(8) .
C6 C7 1.387(7) .
C7 C8 1.409(8) .
C7 C12 1.429(9) .
C8 C9 1.352(9) .
C9 C10 1.391(8) .
C11 C12 1.325(9) .
N3 C13 1.287(6) .
N3 C15 1.503(7) .
N3 Pd 2.027(4) 4
O1 C13 1.330(6) .
O1 C14 1.464(6) .
C14 C17 1.505(7) .
C14 C15 1.552(8) .
C15 C16 1.528(8) .
C17 C22 1.371(8) .
C17 C18 1.402(8) .
C18 C19 1.389(8) .
C19 C20 1.364(8) .
C20 C21 1.380(8) .
C21 C22 1.393(8) .
P1 F3 1.572(5) .
P1 F2 1.588(4) .
P1 F2 1.588(4) 6
P1 F1 1.597(3) .
P1 F1 1.597(3) 6
P1 F4 1.612(5) .
P2 F6 1.548(4) .
P2 F6 1.548(4) 6_655
P2 F7 1.588(4) .
P2 F7 1.588(4) 6_655
P2 F5 1.601(3) 6_655
P2 F5 1.601(3) .
Cl1 C24 1.746(6) .
C24 Cl1 1.746(5) 4
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
_geom_torsion_site_symmetry_1
N3 Pd N1 C1 7.2(5) 4
N2 Pd N1 C1 -179.5(5) .
C23 Pd N1 C1 175.0(14) .
N3 Pd N1 C5 -162.7(3) 4
N2 Pd N1 C5 10.7(3) .
C23 Pd N1 C5 5.2(16) .
N3 Pd N2 C10 -96.5(15) 4
C23 Pd N2 C10 -5.2(5) .
N1 Pd N2 C10 175.5(5) .
N3 Pd N2 C6 78.2(16) 4
C23 Pd N2 C6 169.6(4) .
N1 Pd N2 C6 -9.7(3) .
C5 N1 C1 C2 5.6(7) .
Pd N1 C1 C2 -163.8(4) .
C5 N1 C1 C13 -168.1(5) .
Pd N1 C1 C13 22.5(7) .
N1 C1 C2 C3 -4.6(8) .
C13 C1 C2 C3 169.2(5) .
C1 C2 C3 C4 0.0(8) .
C2 C3 C4 C5 3.1(8) .
C2 C3 C4 C11 -177.9(6) .
C1 N1 C5 C4 -2.2(7) .
Pd N1 C5 C4 169.5(4) .
C1 N1 C5 C6 178.2(4) .
Pd N1 C5 C6 -10.1(5) .
C3 C4 C5 N1 -2.1(8) .
C11 C4 C5 N1 178.9(5) .
C3 C4 C5 C6 177.5(5) .
C11 C4 C5 C6 -1.5(7) .
C10 N2 C6 C7 1.4(7) .
Pd N2 C6 C7 -174.0(4) .
C10 N2 C6 C5 -177.3(5) .
Pd N2 C6 C5 7.3(5) .
N1 C5 C6 N2 2.5(6) .
C4 C5 C6 N2 -177.2(5) .
N1 C5 C6 C7 -176.3(4) .
C4 C5 C6 C7 4.1(7) .
N2 C6 C7 C8 -3.5(8) .
C5 C6 C7 C8 175.1(5) .
N2 C6 C7 C12 178.0(5) .
C5 C6 C7 C12 -3.3(7) .
C6 C7 C8 C9 2.6(8) .
C12 C7 C8 C9 -179.0(6) .
C7 C8 C9 C10 0.3(9) .
C6 N2 C10 C9 1.7(8) .
Pd N2 C10 C9 176.4(4) .
C8 C9 C10 N2 -2.6(9) .
C5 C4 C11 C12 -2.0(9) .
C3 C4 C11 C12 179.1(6) .
C4 C11 C12 C7 2.8(10) .
C6 C7 C12 C11 -0.1(9) .
C8 C7 C12 C11 -178.4(6) .
C15 N3 C13 O1 -4.1(6) .
Pd N3 C13 O1 -176.0(3) 4
C15 N3 C13 C1 168.6(5) .
Pd N3 C13 C1 -3.3(8) 4
C14 O1 C13 N3 -1.4(6) .
C14 O1 C13 C1 -174.8(4) .
N1 C1 C13 N3 46.9(8) .
C2 C1 C13 N3 -127.2(6) .
N1 C1 C13 O1 -140.2(5) .
C2 C1 C13 O1 45.6(7) .
C13 O1 C14 C17 133.3(5) .
C13 O1 C14 C15 5.9(5) .
C13 N3 C15 C16 -116.6(5) .
Pd N3 C15 C16 55.8(5) 4
C13 N3 C15 C14 7.2(5) .
Pd N3 C15 C14 179.6(3) 4
O1 C14 C15 N3 -7.7(5) .
C17 C14 C15 N3 -128.0(5) .
O1 C14 C15 C16 112.4(5) .
C17 C14 C15 C16 -7.9(7) .
O1 C14 C17 C22 -37.4(7) .
C15 C14 C17 C22 81.1(6) .
O1 C14 C17 C18 141.9(5) .
C15 C14 C17 C18 -99.6(6) .
C22 C17 C18 C19 0.7(8) .
C14 C17 C18 C19 -178.6(5) .
C17 C18 C19 C20 -0.3(8) .
C18 C19 C20 C21 -0.4(8) .
C19 C20 C21 C22 0.6(8) .
C18 C17 C22 C21 -0.5(8) .
C14 C17 C22 C21 178.9(5) .
C20 C21 C22 C17 -0.2(8) .
