#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:05:40 +0100 (vie 25 de mar de 2016) $
#$Revision: 179951 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/46/7024652.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_7024652
loop_
_publ_author_name
'Liu, Shaofeng'
'Peloso, Riccardo'
'Braunstein, Pierre'
_publ_section_title
;
 Palladium and iridium complexes with a N,P,N-bis(pyridine)phenylphosphine
 ligand.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2563
_journal_page_last               2572
_journal_paper_doi               10.1039/b919679j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C36 H34 N4 P2 Pd, 2(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C38 H38 B2 Cl4 F8 N4 P2 Pd'
_chemical_formula_weight         1034.48
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 94.187(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0622(6)
_cell_length_b                   10.3296(3)
_cell_length_c                   23.7608(9)
_cell_measurement_reflns_used    5124
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      0.988
_cell_volume                     4421.3(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7367
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.245
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0511
_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)+(0.1005P)²+1.5027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                3379
_reflns_number_total             4331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b919679j.txt
_cod_data_source_block           lsf11
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7024652
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Pd1 Pd 0.5000 0.05564(4) 0.7500 0.02649(18) Uani 1 2 d S
P1 P 0.58600(6) -0.08499(10) 0.72630(5) 0.0264(3) Uani 1 1 d .
N1 N 0.57206(18) 0.1890(3) 0.71493(14) 0.0274(7) Uani 1 1 d .
N2 N 0.5037(2) 0.0133(4) 0.60955(16) 0.0372(9) Uani 1 1 d .
C1 C 0.6662(2) 0.0242(4) 0.7307(2) 0.0342(10) Uani 1 1 d .
H1A H 0.6861 0.0314 0.7696 0.041 Uiso 1 1 calc R
H1B H 0.7047 -0.0103 0.7087 0.041 Uiso 1 1 calc R
C2 C 0.6428(2) 0.1547(4) 0.70881(18) 0.0305(9) Uani 1 1 d .
C3 C 0.6895(3) 0.2365(5) 0.6825(2) 0.0426(12) Uani 1 1 d .
H3 H 0.7388 0.2129 0.6794 0.051 Uiso 1 1 calc R
C4 C 0.6642(3) 0.3522(5) 0.6610(2) 0.0493(13) Uani 1 1 d .
H4 H 0.6960 0.4087 0.6442 0.059 Uiso 1 1 calc R
C5 C 0.5895(3) 0.3842(4) 0.6648(2) 0.0416(11) Uani 1 1 d .
H5 H 0.5702 0.4608 0.6493 0.050 Uiso 1 1 calc R
C6 C 0.5457(3) 0.3009(4) 0.69159(19) 0.0360(10) Uani 1 1 d .
H6 H 0.4959 0.3214 0.6940 0.043 Uiso 1 1 calc R
C7 C 0.5793(2) -0.1532(4) 0.65565(17) 0.0311(9) Uani 1 1 d .
H7A H 0.6243 -0.2010 0.6498 0.037 Uiso 1 1 calc R
H7B H 0.5380 -0.2133 0.6520 0.037 Uiso 1 1 calc R
C8 C 0.5682(2) -0.0495(4) 0.61107(18) 0.0309(9) Uani 1 1 d .
C9 C 0.6227(3) -0.0202(5) 0.5751(2) 0.0500(13) Uani 1 1 d .
H9 H 0.6673 -0.0656 0.5770 0.060 Uiso 1 1 calc R
C10 C 0.6094(4) 0.0780(6) 0.5363(3) 0.0614(16) Uani 1 1 d .
H10 H 0.6451 0.0997 0.5117 0.074 Uiso 1 1 calc R
C11 C 0.5441(3) 0.1426(5) 0.5342(2) 0.0546(14) Uani 1 1 d .
H11 H 0.5343 0.2090 0.5083 0.065 Uiso 1 1 calc R
C12 C 0.4924(3) 0.1075(5) 0.5716(2) 0.0477(12) Uani 1 1 d .
H12 H 0.4475 0.1519 0.5701 0.057 Uiso 1 1 calc R
C13 C 0.6056(2) -0.2156(4) 0.77568(18) 0.0307(9) Uani 1 1 d .
C14 C 0.6108(2) -0.3444(4) 0.7587(2) 0.0386(11) Uani 1 1 d .
H14 H 0.6067 -0.3650 0.7205 0.046 Uiso 1 1 calc R
C15 C 0.6222(3) -0.4415(4) 0.7985(2) 0.0451(12) Uani 1 1 d .
H15 H 0.6259 -0.5272 0.7871 0.054 Uiso 1 1 calc R
C16 C 0.6280(3) -0.4113(5) 0.8546(2) 0.0482(13) Uani 1 1 d .
H16 H 0.6350 -0.4769 0.8813 0.058 Uiso 1 1 calc R
C17 C 0.6234(3) -0.2828(5) 0.8724(2) 0.0473(12) Uani 1 1 d .
H17 H 0.6280 -0.2627 0.9107 0.057 Uiso 1 1 calc R
C18 C 0.6121(2) -0.1865(5) 0.83281(19) 0.0387(11) Uani 1 1 d .
H18 H 0.6088 -0.1009 0.8444 0.046 Uiso 1 1 calc R
C19 C 0.6732(5) -0.4276(7) 0.5197(3) 0.093(3) Uani 1 1 d .
H19A H 0.7053 -0.3907 0.5501 0.111 Uiso 1 1 calc R
H19B H 0.6827 -0.3822 0.4852 0.111 Uiso 1 1 calc R
B1 B 0.7977(3) -0.2743(5) 0.6402(2) 0.0377(12) Uani 1 1 d .
F1 F 0.7843(3) -0.2149(4) 0.59017(17) 0.1055(15) Uani 1 1 d .
F2 F 0.7774(3) -0.3976(4) 0.63633(19) 0.136(2) Uani 1 1 d .
F3 F 0.86863(17) -0.2631(4) 0.66162(15) 0.0785(11) Uani 1 1 d .
F4 F 0.7566(3) -0.2164(6) 0.6788(2) 0.139(2) Uani 1 1 d .
Cl1 Cl 0.58251(19) -0.4039(3) 0.53378(14) 0.1526(12) Uani 1 1 d .
Cl2 Cl 0.69505(12) -0.5910(2) 0.51233(8) 0.0920(6) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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
N1 Pd1 N1 98.38(18) 2_656 .
N1 Pd1 P1 82.21(9) 2_656 2_656
N1 Pd1 P1 170.93(10) . 2_656
N1 Pd1 P1 170.93(10) 2_656 .
N1 Pd1 P1 82.21(9) . .
P1 Pd1 P1 98.65(6) 2_656 .
C13 P1 C7 107.91(19) . .
C13 P1 C1 107.8(2) . .
C7 P1 C1 106.9(2) . .
C13 P1 Pd1 115.47(14) . .
C7 P1 Pd1 119.03(14) . .
C1 P1 Pd1 98.43(14) . .
C2 N1 C6 119.3(4) . .
C2 N1 Pd1 119.3(3) . .
C6 N1 Pd1 120.8(3) . .
C8 N2 C12 117.6(4) . .
C2 C1 P1 109.5(3) . .
C2 C1 H1A 109.8 . .
P1 C1 H1A 109.8 . .
C2 C1 H1B 109.8 . .
P1 C1 H1B 109.8 . .
H1A C1 H1B 108.2 . .
N1 C2 C3 120.4(4) . .
N1 C2 C1 116.5(3) . .
C3 C2 C1 123.1(4) . .
C4 C3 C2 120.5(5) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
C3 C4 C5 118.7(4) . .
C3 C4 H4 120.6 . .
C5 C4 H4 120.6 . .
C6 C5 C4 118.6(4) . .
C6 C5 H5 120.7 . .
C4 C5 H5 120.7 . .
N1 C6 C5 122.3(4) . .
N1 C6 H6 118.9 . .
C5 C6 H6 118.9 . .
C8 C7 P1 111.7(3) . .
C8 C7 H7A 109.3 . .
P1 C7 H7A 109.3 . .
C8 C7 H7B 109.3 . .
P1 C7 H7B 109.3 . .
H7A C7 H7B 107.9 . .
N2 C8 C9 122.5(4) . .
N2 C8 C7 115.8(4) . .
C9 C8 C7 121.7(4) . .
C10 C9 C8 118.4(5) . .
C10 C9 H9 120.8 . .
C8 C9 H9 120.8 . .
C11 C10 C9 119.8(5) . .
C11 C10 H10 120.1 . .
C9 C10 H10 120.1 . .
C10 C11 C12 118.3(5) . .
C10 C11 H11 120.8 . .
C12 C11 H11 120.8 . .
N2 C12 C11 123.3(5) . .
N2 C12 H12 118.3 . .
C11 C12 H12 118.3 . .
C18 C13 C14 119.2(4) . .
C18 C13 P1 118.2(3) . .
C14 C13 P1 122.5(3) . .
C15 C14 C13 120.1(4) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C16 C15 C14 120.0(4) . .
C16 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
C15 C16 C17 120.7(4) . .
C15 C16 H16 119.6 . .
C17 C16 H16 119.6 . .
C18 C17 C16 119.3(5) . .
C18 C17 H17 120.4 . .
C16 C17 H17 120.4 . .
C17 C18 C13 120.7(4) . .
C17 C18 H18 119.6 . .
C13 C18 H18 119.6 . .
Cl1 C19 Cl2 112.6(4) . .
Cl1 C19 H19A 109.1 . .
Cl2 C19 H19A 109.1 . .
Cl1 C19 H19B 109.1 . .
Cl2 C19 H19B 109.1 . .
H19A C19 H19B 107.8 . .
F2 B1 F1 110.2(5) . .
F2 B1 F3 111.0(5) . .
F1 B1 F3 113.6(5) . .
F2 B1 F4 107.9(5) . .
F1 B1 F4 108.9(5) . .
F3 B1 F4 105.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.108(3) 2_656
Pd1 N1 2.108(3) .
Pd1 P1 2.2289(11) 2_656
Pd1 P1 2.2289(11) .
P1 C13 1.806(4) .
P1 C7 1.816(4) .
P1 C1 1.832(4) .
N1 C2 1.345(5) .
N1 C6 1.353(5) .
N2 C8 1.332(6) .
N2 C12 1.333(6) .
C1 C2 1.495(6) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.375(6) .
C3 C4 1.366(7) .
C3 H3 0.9300 .
C4 C5 1.399(7) .
C4 H4 0.9300 .
C5 C6 1.358(6) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.509(6) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.384(7) .
C9 C10 1.379(7) .
C9 H9 0.9300 .
C10 C11 1.352(8) .
C10 H10 0.9300 .
C11 C12 1.383(7) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 C18 1.387(6) .
C13 C14 1.396(6) .
C14 C15 1.384(6) .
C14 H14 0.9300 .
C15 C16 1.366(7) .
C15 H15 0.9300 .
C16 C17 1.397(7) .
C16 H16 0.9300 .
C17 C18 1.375(6) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 Cl1 1.713(10) .
C19 Cl2 1.745(8) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
B1 F2 1.327(6) .
B1 F1 1.344(6) .
B1 F3 1.348(6) .
B1 F4 1.359(7) .
