#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/43/2014347.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_2014347
loop_
_publ_author_name
'Magno Agostinho'
'Andrei Banu'
'Pierre Braunstein'
'Richard Welter'
'Xavier Morise'
_publ_section_title
;
 New palladium complexes with phosphino- and phosphinitopyridine
 ligands
;
_journal_coeditor_code           GG1299
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m81
_journal_page_last               m86
_journal_paper_doi               10.1107/S0108270106001296
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C26 H24 Cl2 N P Pd'
_chemical_formula_moiety         '[Pd Cl2 (C26 H24 N P)]'
_chemical_formula_sum            'C26 H24 Cl2 N P Pd'
_chemical_formula_weight         558.73
_chemical_name_systematic
;
dichloro[2-(2,6-dimethylphenyl)-6-(diphenylphosphanomethyl)pyridine-
κ²N,P]palladium(II)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.40(5)
_cell_angle_beta                 109.93(5)
_cell_angle_gamma                112.23(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1510(10)
_cell_length_b                   11.4610(10)
_cell_length_c                   12.106(2)
_cell_measurement_reflns_used    7840
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.998
_cell_volume                     1184.7(9)
_computing_cell_refinement       'Denzo (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        Denzo
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ or ω scans?'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14956
_diffrn_reflns_theta_full        27.82
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow--orange
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.801
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0305
_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)+(0.0331P)²+0.3488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                4878
_reflns_number_total             5587
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gg1299.cif
_cod_data_source_block           IV
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (7 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (7
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2014347
_cod_database_fobs_code          2014347
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_disorder_assembly
_atom_site_disorder_group
Pd Pd1 0.194666(18) -0.044011(15) 0.279218(15) 0.02745(7) Uani d . 1 . .
Cl Cl1 0.09907(8) -0.27189(5) 0.26100(6) 0.04143(16) Uani d . 1 . .
Cl Cl2 -0.03851(7) -0.04876(6) 0.25935(7) 0.04838(17) Uani d . 1 . .
P P1 0.30688(7) 0.17127(5) 0.33743(5) 0.02879(14) Uani d . 1 . .
N N1 0.4199(2) -0.01187(17) 0.29826(16) 0.0270(4) Uani d . 1 . .
C C1 0.4896(3) 0.1836(2) 0.4487(2) 0.0336(5) Uani d . 1 . .
H H1A 0.5711 0.2748 0.4758 0.040 Uiso calc . 1 . .
H H1B 0.4749 0.1565 0.5205 0.040 Uiso calc . 1 . .
C C2 0.5374(3) 0.0955(2) 0.3882(2) 0.0301(5) Uani d . 1 . .
C C3 0.6920(3) 0.1252(2) 0.4180(2) 0.0391(6) Uani d . 1 . .
H H3 0.7716 0.1993 0.4818 0.047 Uiso calc . 1 . .
C C4 0.7299(3) 0.0469(3) 0.3548(2) 0.0445(6) Uani d . 1 . .
H H4 0.8359 0.0645 0.3757 0.053 Uiso calc . 1 . .
C C5 0.6123(3) -0.0581(2) 0.2603(2) 0.0391(6) Uani d . 1 . .
H H5 0.6378 -0.1118 0.2149 0.047 Uiso calc . 1 . .
C C6 0.4565(3) -0.0860(2) 0.2308(2) 0.0297(5) Uani d . 1 . .
C C7 0.3342(3) -0.1896(2) 0.1182(2) 0.0311(5) Uani d . 1 . .
C C8 0.3001(3) -0.3211(2) 0.1115(2) 0.0380(6) Uani d . 1 . .
C C9 0.1895(3) -0.4132(2) 0.0021(3) 0.0482(7) Uani d . 1 . .
H H9 0.1623 -0.5032 -0.0034 0.058 Uiso calc . 1 . .
C C10 0.1196(3) -0.3756(3) -0.0973(3) 0.0533(8) Uani d . 1 . .
H H10 0.0436 -0.4397 -0.1705 0.064 Uiso calc . 1 . .
C C11 0.1589(3) -0.2464(3) -0.0915(2) 0.0479(7) Uani d . 1 . .
H H11 0.1126 -0.2216 -0.1620 0.057 Uiso calc . 1 . .
C C12 0.2653(3) -0.1508(2) 0.0157(2) 0.0368(5) Uani d . 1 . .
C C13 0.3741(4) -0.3664(3) 0.2176(3) 0.0534(7) Uani d . 1 . .
H H13A 0.3389 -0.3514 0.2812 0.080 Uiso calc . 1 . .
H H13B 0.4878 -0.3177 0.2496 0.080 Uiso calc . 1 . .
H H13C 0.3439 -0.4597 0.1913 0.080 Uiso calc . 1 . .
C C14 0.3075(4) -0.0112(3) 0.0163(3) 0.0551(8) Uani d . 1 . .
H H14A 0.2941 -0.0006 -0.0657 0.083 Uiso calc . 1 . .
H H14B 0.4164 0.0425 0.0730 0.083 Uiso calc . 1 . .
H H14C 0.2397 0.0163 0.0418 0.083 Uiso calc . 1 . .
C C15 0.2380(3) 0.2622(2) 0.4158(2) 0.0323(5) Uani d . 1 . .
C C16 0.2256(3) 0.3718(2) 0.3845(2) 0.0431(6) Uani d . 1 . .
H H16 0.2537 0.4006 0.3212 0.052 Uiso calc . 1 . .
C C17 0.1720(4) 0.4398(3) 0.4452(3) 0.0520(7) Uani d . 1 . .
H H17 0.1624 0.5145 0.4230 0.062 Uiso calc . 1 . .
C C18 0.1328(3) 0.3988(3) 0.5378(3) 0.0516(7) Uani d . 1 . .
H H18 0.0963 0.4454 0.5794 0.062 Uiso calc . 1 . .
C C19 0.1462(3) 0.2907(3) 0.5704(3) 0.0500(7) Uani d . 1 . .
H H19 0.1207 0.2638 0.6352 0.060 Uiso calc . 1 . .
C C20 0.1967(3) 0.2210(2) 0.5088(2) 0.0404(6) Uani d . 1 . .
H H20 0.2032 0.1450 0.5299 0.049 Uiso calc . 1 . .
C C21 0.3442(3) 0.2497(2) 0.2223(2) 0.0333(5) Uani d . 1 . .
C C22 0.4934(3) 0.3177(3) 0.2287(3) 0.0516(7) Uani d . 1 . .
H H22 0.5819 0.3328 0.2996 0.062 Uiso calc . 1 . .
C C23 0.5120(5) 0.3636(3) 0.1300(4) 0.0724(10) Uani d . 1 . .
H H23 0.6139 0.4099 0.1337 0.087 Uiso calc . 1 . .
C C24 0.3865(5) 0.3430(3) 0.0286(3) 0.0689(10) Uani d . 1 . .
H H24 0.4013 0.3731 -0.0386 0.083 Uiso calc . 1 . .
C C25 0.2390(4) 0.2793(3) 0.0223(3) 0.0601(9) Uani d . 1 . .
H H25 0.1518 0.2681 -0.0480 0.072 Uiso calc . 1 . .
C C26 0.2166(3) 0.2311(2) 0.1187(2) 0.0434(6) Uani d . 1 . .
H H26 0.1140 0.1854 0.1138 0.052 Uiso calc . 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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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_publ_flag
N1 Pd1 P1 81.74(5) y
N1 Pd1 Cl2 171.99(5) y
P1 Pd1 Cl2 90.52(3) y
N1 Pd1 Cl1 96.05(5) y
P1 Pd1 Cl1 167.92(2) y
Cl2 Pd1 Cl1 91.95(3) y
C21 P1 C15 107.09(11) ?
C21 P1 C1 109.32(11) ?
C15 P1 C1 107.36(11) ?
C21 P1 Pd1 114.41(8) ?
C15 P1 Pd1 122.56(8) ?
C1 P1 Pd1 94.68(8) ?
C6 N1 C2 119.13(19) ?
C6 N1 Pd1 126.31(15) ?
C2 N1 Pd1 114.56(14) ?
C2 C1 P1 107.59(15) ?
C2 C1 H1A 110.2 ?
P1 C1 H1A 110.2 ?
C2 C1 H1B 110.2 ?
P1 C1 H1B 110.2 ?
H1A C1 H1B 108.5 ?
N1 C2 C3 121.8(2) ?
N1 C2 C1 116.7(2) ?
C3 C2 C1 121.4(2) ?
C4 C3 C2 119.3(2) ?
C4 C3 H3 120.3 ?
C2 C3 H3 120.3 ?
C3 C4 C5 119.2(2) ?
C3 C4 H4 120.4 ?
C5 C4 H4 120.4 ?
C4 C5 C6 120.7(2) ?
C4 C5 H5 119.7 ?
C6 C5 H5 119.7 ?
N1 C6 C5 119.7(2) ?
N1 C6 C7 121.3(2) ?
C5 C6 C7 118.7(2) ?
C8 C7 C12 120.8(2) ?
C8 C7 C6 120.7(2) ?
C12 C7 C6 118.2(2) ?
C9 C8 C7 118.2(2) ?
C9 C8 C13 119.2(2) ?
C7 C8 C13 122.6(2) ?
C10 C9 C8 121.0(2) ?
C10 C9 H9 119.5 ?
C8 C9 H9 119.5 ?
C11 C10 C9 120.3(2) ?
C11 C10 H10 119.8 ?
C9 C10 H10 119.8 ?
C10 C11 C12 121.2(3) ?
C10 C11 H11 119.4 ?
C12 C11 H11 119.4 ?
C11 C12 C7 118.4(2) ?
C11 C12 C14 119.0(2) ?
C7 C12 C14 122.5(2) ?
C8 C13 H13A 109.5 ?
C8 C13 H13B 109.5 ?
H13A C13 H13B 109.5 ?
C8 C13 H13C 109.5 ?
H13A C13 H13C 109.5 ?
H13B C13 H13C 109.5 ?
C12 C14 H14A 109.5 ?
C12 C14 H14B 109.5 ?
H14A C14 H14B 109.5 ?
C12 C14 H14C 109.5 ?
H14A C14 H14C 109.5 ?
H14B C14 H14C 109.5 ?
C16 C15 C20 119.4(2) ?
C16 C15 P1 121.09(18) ?
C20 C15 P1 119.53(19) ?
C15 C16 C17 120.2(2) ?
C15 C16 H16 119.9 ?
C17 C16 H16 119.9 ?
C18 C17 C16 119.8(3) ?
C18 C17 H17 120.1 ?
C16 C17 H17 120.1 ?
C19 C18 C17 120.4(2) ?
C19 C18 H18 119.8 ?
C17 C18 H18 119.8 ?
C18 C19 C20 120.1(3) ?
C18 C19 H19 120.0 ?
C20 C19 H19 120.0 ?
C19 C20 C15 120.1(2) ?
C19 C20 H20 120.0 ?
C15 C20 H20 120.0 ?
C22 C21 C26 119.4(2) ?
C22 C21 P1 122.7(2) ?
C26 C21 P1 117.74(18) ?
C21 C22 C23 119.2(3) ?
C21 C22 H22 120.4 ?
C23 C22 H22 120.4 ?
C24 C23 C22 120.8(3) ?
C24 C23 H23 119.6 ?
C22 C23 H23 119.6 ?
C23 C24 C25 120.7(3) ?
C23 C24 H24 119.7 ?
C25 C24 H24 119.7 ?
C24 C25 C26 119.8(3) ?
C24 C25 H25 120.1 ?
C26 C25 H25 120.1 ?
C25 C26 C21 120.0(3) ?
C25 C26 H26 120.0 ?
C21 C26 H26 120.0 ?
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 Cl1 . 2.3747(12) y
Pd1 Cl2 . 2.2749(13) y
Pd1 P1 . 2.2093(11) y
Pd1 N1 . 2.098(2) y
P1 C21 . 1.798(2) ?
P1 C15 . 1.814(2) ?
P1 C1 . 1.826(3) y
N1 C6 . 1.357(3) ?
N1 C2 . 1.369(3) y
C1 C2 . 1.506(3) y
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 C3 . 1.378(3) ?
C3 C4 . 1.368(4) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.380(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.393(3) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.496(3) ?
C7 C8 . 1.400(3) ?
C7 C12 . 1.405(3) ?
C8 C9 . 1.398(4) ?
C8 C13 . 1.499(4) ?
C9 C10 . 1.373(4) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.368(4) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.391(4) ?
C11 H11 . 0.9500 ?
C12 C14 . 1.490(4) ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C13 H13C . 0.9800 ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
C15 C16 . 1.383(3) ?
C15 C20 . 1.392(3) ?
C16 C17 . 1.390(4) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.377(4) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.375(4) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.384(4) ?
C19 H19 . 0.9500 ?
C20 H20 . 0.9500 ?
C21 C22 . 1.387(4) ?
C21 C26 . 1.389(4) ?
C22 C23 . 1.392(4) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.355(5) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.366(5) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.388(4) ?
C25 H25 . 0.9500 ?
C26 H26 . 0.9500 ?
