#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:31:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179794 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/90/7009008.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_7009008
loop_
_publ_author_name
'Dervisi, Athanasia'
'Edwards, Peter G.'
'Newman, Paul D.'
'Tooze, Robert P.'
_publ_section_title
;
 Synthesis and chemistry of diphenyl-2-pyridylphosphine complexes of
 palladium(0). X-Ray characterisation of Pd(Ph2Ppy)2(η2-DMAD) and
 trans-Pd(Ph2Ppy)2(PhCCH2)(CF3CO2)
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              523
_journal_paper_doi               10.1039/a908050c
_journal_year                    2000
_chemical_formula_sum            'C44 H35 F3 N2 O2 P2 Pd'
_chemical_formula_weight         849.08
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                95.32(7)
_cell_angle_beta                 103.28(2)
_cell_angle_gamma                110.28(3)
_cell_formula_units_Z            2
_cell_length_a                   11.837(2)
_cell_length_b                   13.342(7)
_cell_length_c                   13.729(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1943.8(14)
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0827
_diffrn_reflns_av_sigmaI/netI    0.5634
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7136
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.614
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_F_000             864
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.437
_refine_ls_goodness_of_fit_obs   0.645
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         5013
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.511
_refine_ls_restrained_S_obs      0.797
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_obs          0.0397
_refine_ls_shift/esd_max         7.713
_refine_ls_shift/esd_mean        0.125
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0740
_refine_ls_wR_factor_obs         0.0587
_reflns_number_observed          1828
_reflns_number_total             5014
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908050c.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1943.8(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009008
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd1 Pd 0.72618(7) 0.76810(6) 0.69956(5) 0.0416(2) Uani 1 d . .
P1 P 0.9081(2) 0.7633(2) 0.66436(13) 0.0393(6) Uani 1 d . .
P2 P 0.5720(2) 0.8235(2) 0.73979(13) 0.0429(6) Uani 1 d . .
N1 N 0.9542(7) 0.8377(6) 0.4867(5) 0.085(3) Uani 1 d . .
N2 N 0.5995(8) 1.0395(7) 0.7423(5) 0.076(2) Uani 1 d . .
F1 F 0.7677(29) 0.5314(15) 0.9282(13) 0.129(12) Uani 0.59(4) d P 1
F1' F 0.7190(48) 0.5586(41) 0.9647(29) 0.184(26) Uani 0.41(4) d P 2
F2 F 0.9256(17) 0.6457(16) 1.0237(20) 0.148(13) Uani 0.59(4) d P 1
F2' F 0.8689(71) 0.5631(64) 0.9526(59) 0.787(73) Uani 0.41(4) d P 2
F3 F 0.7501(27) 0.6488(22) 1.0414(18) 0.131(11) Uani 0.59(4) d P 1
F3' F 0.8513(52) 0.6664(34) 1.0609(22) 0.211(23) Uani 0.41(4) d P 2
O1 O 0.7393(5) 0.6722(4) 0.8148(3) 0.058(2) Uani 1 d . .
O2 O 0.8753(7) 0.8044(5) 0.9317(4) 0.093(2) Uani 1 d . .
C1 C 0.9086(7) 0.7429(7) 0.5303(5) 0.042(2) Uani 1 d . .
C2 C 0.8511(7) 0.6400(7) 0.4720(5) 0.053(2) Uani 1 d . .
H2 H 0.8200(7) 0.5803(7) 0.5019(5) 0.064 Uiso 1 calc R .
C3 C 0.8399(8) 0.6258(7) 0.3683(6) 0.073(3) Uani 1 d . .
H3 H 0.8039(8) 0.5560(7) 0.3290(6) 0.087 Uiso 1 calc R .
C4 C 0.8812(9) 0.7130(9) 0.3237(6) 0.075(3) Uani 1 d . .
H4 H 0.8712(9) 0.7019(9) 0.2539(6) 0.091 Uiso 1 calc R .
C5 C 0.9374(8) 0.8168(8) 0.3791(6) 0.069(3) Uani 1 d . .
H5 H 0.9651(8) 0.8747(8) 0.3463(6) 0.083 Uiso 1 calc R .
C6 C 0.9498(8) 0.6554(7) 0.7155(5) 0.043(2) Uani 1 d . .
C7 C 0.8639(8) 0.5564(7) 0.6843(5) 0.049(2) Uani 1 d . .
H7 H 0.7892(8) 0.5441(7) 0.6355(5) 0.058 Uiso 1 calc R .
C8 C 0.8835(10) 0.4735(7) 0.7224(6) 0.079(3) Uani 1 d . .
H8 H 0.8216(10) 0.4041(7) 0.6987(6) 0.095 Uiso 1 calc R .
C9 C 0.9894(11) 0.4865(8) 0.7938(7) 0.084(3) Uani 1 d . .
H9 H 0.9999(11) 0.4277(8) 0.8205(7) 0.101 Uiso 1 calc R .
C10 C 1.0791(10) 0.5863(9) 0.8251(7) 0.092(4) Uani 1 d . .
H10 H 1.1540(10) 0.5973(9) 0.8729(7) 0.111 Uiso 1 calc R .
C11 C 1.0603(8) 0.6738(7) 0.7862(6) 0.071(3) Uani 1 d . .
H11 H 1.1220(8) 0.7435(7) 0.8079(6) 0.086 Uiso 1 calc R .
C12 C 1.0435(7) 0.8886(6) 0.7266(5) 0.040(2) Uani 1 d . .
C13 C 1.1596(8) 0.9093(7) 0.7075(6) 0.059(3) Uani 1 d . .
H13 H 1.1682(8) 0.8623(7) 0.6577(6) 0.071 Uiso 1 calc R .
C14 C 1.2615(8) 1.0002(8) 0.7634(7) 0.073(3) Uani 1 d . .
H14 H 1.3397(8) 1.0145(8) 0.7522(7) 0.088 Uiso 1 calc R .
C15 C 1.2469(10) 1.0709(8) 0.8371(6) 0.083(4) Uani 1 d . .
H15 H 1.3151(10) 1.1332(8) 0.8733(6) 0.100 Uiso 1 calc R .
C16 C 1.1354(9) 1.0495(7) 0.8559(6) 0.075(3) Uani 1 d . .
H16 H 1.1267(9) 1.0957(7) 0.9061(6) 0.089 Uiso 1 calc R .
C17 C 1.0339(8) 0.9582(7) 0.8000(5) 0.053(2) Uani 1 d . .
H17 H 0.9566(8) 0.9440(7) 0.8130(5) 0.064 Uiso 1 calc R .
C18 C 0.8109(8) 0.7190(7) 0.8963(6) 0.040(2) Uani 1 d U .
C19 C 0.8218(18) 0.6336(12) 0.9734(10) 0.088(5) Uani 1 d . .
C20 C 0.7009(7) 0.8359(6) 0.5767(5) 0.034(2) Uani 1 d . .
C21 C 0.7556(7) 0.9423(6) 0.5813(5) 0.046(2) Uani 1 d . .
H21A H 0.7470(7) 0.9710(6) 0.5221(5) 0.055 Uiso 1 calc R .
H21B H 0.8026(7) 0.9880(6) 0.6437(5) 0.055 Uiso 1 calc R .
C22 C 0.6245(7) 0.7584(6) 0.4792(5) 0.042(2) Uani 1 d . .
C23 C 0.6320(8) 0.7834(7) 0.3840(6) 0.069(3) Uani 1 d . .
H23 H 0.6874(8) 0.8513(7) 0.3804(6) 0.083 Uiso 1 calc R .
C24 C 0.5604(10) 0.7109(9) 0.2957(6) 0.085(3) Uani 1 d . .
H24 H 0.5668(10) 0.7310(9) 0.2336(6) 0.102 Uiso 1 calc R .
C25 C 0.4803(10) 0.6104(8) 0.2971(7) 0.085(3) Uani 1 d . .
H25 H 0.4350(10) 0.5606(8) 0.2366(7) 0.102 Uiso 1 calc R .
C26 C 0.4667(8) 0.5826(7) 0.3896(7) 0.082(3) Uani 1 d . .
H26 H 0.4100(8) 0.5147(7) 0.3919(7) 0.098 Uiso 1 calc R .
C27 C 0.5389(8) 0.6574(7) 0.4790(5) 0.063(3) Uani 1 d . .
H27 H 0.5290(8) 0.6385(7) 0.5410(5) 0.076 Uiso 1 calc R .
C28 C 0.5136(8) 0.7769(8) 0.8461(6) 0.049(3) Uani 1 d . .
C29 C 0.4991(8) 0.6744(8) 0.8636(6) 0.082(3) Uani 1 d . .
H29 H 0.5257(8) 0.6315(8) 0.8242(6) 0.098 Uiso 1 calc R .
C30 C 0.4454(10) 0.6326(10) 0.9391(8) 0.118(5) Uani 1 d . .
H30 H 0.4336(10) 0.5620(10) 0.9488(8) 0.141 Uiso 1 calc R .
C31 C 0.4113(9) 0.6973(10) 0.9972(7) 0.088(4) Uani 1 d . .
H31 H 0.3804(9) 0.6720(10) 1.0504(7) 0.106 Uiso 1 calc R .
C32 C 0.4207(9) 0.8011(9) 0.9806(6) 0.088(4) Uani 1 d . .
H32 H 0.3922(9) 0.8434(9) 1.0188(6) 0.106 Uiso 1 calc R .
C33 C 0.4757(8) 0.8389(7) 0.9030(5) 0.068(3) Uani 1 d . .
H33 H 0.4857(8) 0.9086(7) 0.8912(5) 0.082 Uiso 1 calc R .
C34 C 0.6475(8) 0.9699(6) 0.7855(6) 0.048(2) Uani 1 d . .
C35 C 0.6688(11) 1.1496(8) 0.7797(7) 0.082(3) Uani 1 d . .
H35 H 0.6397(11) 1.1996(8) 0.7511(7) 0.099 Uiso 1 calc R .
C36 C 0.7793(10) 1.1880(8) 0.8575(7) 0.082(3) Uani 1 d . .
H36 H 0.8229(10) 1.2626(8) 0.8799(7) 0.098 Uiso 1 calc R .
C37 C 0.8250(8) 1.1169(8) 0.9021(6) 0.069(3) Uani 1 d . .
H37 H 0.8983(8) 1.1417(8) 0.9556(6) 0.083 Uiso 1 calc R .
C38 C 0.7587(8) 1.0082(7) 0.8650(6) 0.059(2) Uani 1 d . .
H38 H 0.7885(8) 0.9584(7) 0.8934(6) 0.071 Uiso 1 calc R .
C39 C 0.4272(7) 0.7946(7) 0.6407(5) 0.046(2) Uani 1 d . .
C40 C 0.4203(8) 0.8515(7) 0.5623(5) 0.062(3) Uani 1 d . .
H40 H 0.4906(8) 0.9108(7) 0.5619(5) 0.074 Uiso 1 calc R .
C41 C 0.3125(11) 0.8226(8) 0.4850(6) 0.077(3) Uani 1 d . .
H41 H 0.3104(11) 0.8615(8) 0.4323(6) 0.093 Uiso 1 calc R .
C42 C 0.2072(10) 0.7360(10) 0.4848(7) 0.084(4) Uani 1 d . .
H42 H 0.1336(10) 0.7167(10) 0.4324(7) 0.101 Uiso 1 calc R .
C43 C 0.2111(9) 0.6786(8) 0.5621(7) 0.081(3) Uani 1 d . .
H43 H 0.1403(9) 0.6199(8) 0.5627(7) 0.098 Uiso 1 calc R .
C44 C 0.3212(8) 0.7085(7) 0.6393(5) 0.064(3) Uani 1 d . .
H44 H 0.3234(8) 0.6693(7) 0.6918(5) 0.077 Uiso 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'
F F 0.0171 0.0103 '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'
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
C20 Pd1 O1 171.2(3) . . ?
C20 Pd1 P1 86.8(2) . . ?
O1 Pd1 P1 92.3(2) . . ?
C20 Pd1 P2 85.9(2) . . ?
O1 Pd1 P2 96.9(2) . . ?
P1 Pd1 P2 164.56(8) . . ?
C6 P1 C12 104.8(4) . . ?
C6 P1 C1 105.0(4) . . ?
C12 P1 C1 105.3(4) . . ?
C6 P1 Pd1 111.3(3) . . ?
C12 P1 Pd1 111.3(3) . . ?
C1 P1 Pd1 118.0(3) . . ?
C34 P2 C39 108.7(4) . . ?
C34 P2 C28 101.9(4) . . ?
C39 P2 C28 102.0(4) . . ?
C34 P2 Pd1 105.9(3) . . ?
C39 P2 Pd1 118.6(3) . . ?
C28 P2 Pd1 118.2(3) . . ?
C5 N1 C1 115.2(7) . . ?
C34 N2 C35 116.2(9) . . ?
C18 O1 Pd1 116.5(6) . . ?
C2 C1 N1 122.0(6) . . ?
C2 C1 P1 119.4(6) . . ?
N1 C1 P1 118.0(6) . . ?
C1 C2 C3 119.6(7) . . ?
C4 C3 C2 120.4(8) . . ?
C3 C4 C5 121.6(8) . . ?
C4 C5 N1 121.1(8) . . ?
C7 C6 C11 120.2(8) . . ?
C7 C6 P1 116.2(7) . . ?
C11 C6 P1 123.6(7) . . ?
C6 C7 C8 120.2(8) . . ?
C7 C8 C9 122.6(9) . . ?
C10 C9 C8 118.1(10) . . ?
C9 C10 C11 120.1(10) . . ?
C6 C11 C10 118.8(9) . . ?
C17 C12 C13 119.2(8) . . ?
C17 C12 P1 119.0(6) . . ?
C13 C12 P1 121.5(7) . . ?
C14 C13 C12 119.1(8) . . ?
C13 C14 C15 119.8(9) . . ?
C16 C15 C14 120.6(10) . . ?
C15 C16 C17 119.4(10) . . ?
C12 C17 C16 121.9(9) . . ?
O2 C18 O1 136.4(10) . . ?
O2 C18 C19 112.3(9) . . ?
O1 C18 C19 111.1(9) . . ?
F2' C19 F3' 111.3(37) . . ?
F2 C19 F1 106.4(24) . . ?
F2' C19 F1' 90.3(38) . . ?
F3' C19 F1' 99.5(30) . . ?
F2 C19 F3 108.7(23) . . ?
F1 C19 F3 106.1(21) . . ?
F2' C19 C18 119.3(25) . . ?
F3' C19 C18 118.0(20) . . ?
F2 C19 C18 117.5(14) . . ?
F1 C19 C18 113.7(13) . . ?
F1' C19 C18 113.1(21) . . ?
F3 C19 C18 103.7(14) . . ?
C21 C20 C22 122.6(6) . . ?
C21 C20 Pd1 121.8(6) . . ?
C22 C20 Pd1 115.4(5) . . ?
C27 C22 C23 116.1(7) . . ?
C27 C22 C20 120.7(7) . . ?
C23 C22 C20 123.1(7) . . ?
C24 C23 C22 121.9(8) . . ?
C25 C24 C23 121.2(9) . . ?
C24 C25 C26 119.2(8) . . ?
C25 C26 C27 119.1(8) . . ?
C22 C27 C26 122.4(8) . . ?
C33 C28 C29 119.2(8) . . ?
C33 C28 P2 120.6(8) . . ?
C29 C28 P2 120.0(7) . . ?
C28 C29 C30 121.7(10) . . ?
C31 C30 C29 118.1(12) . . ?
C30 C31 C32 122.4(11) . . ?
C31 C32 C33 116.8(10) . . ?
C28 C33 C32 121.7(9) . . ?
N2 C34 C38 121.3(8) . . ?
N2 C34 P2 121.3(7) . . ?
C38 C34 P2 117.3(7) . . ?
C36 C35 N2 122.8(10) . . ?
C37 C36 C35 120.4(10) . . ?
C38 C37 C36 117.5(9) . . ?
C37 C38 C34 121.8(9) . . ?
C44 C39 C40 117.7(8) . . ?
C44 C39 P2 119.4(6) . . ?
C40 C39 P2 122.8(7) . . ?
C41 C40 C39 121.3(9) . . ?
C42 C41 C40 120.2(9) . . ?
C41 C42 C43 119.6(9) . . ?
C42 C43 C44 119.4(10) . . ?
C39 C44 C43 121.7(8) . . ?
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 C20 1.998(6) . ?
Pd1 O1 2.136(5) . ?
Pd1 P1 2.334(2) . ?
Pd1 P2 2.346(2) . ?
P1 C6 1.824(8) . ?
P1 C12 1.829(7) . ?
P1 C1 1.837(7) . ?
P2 C34 1.820(8) . ?
P2 C39 1.820(7) . ?
P2 C28 1.825(7) . ?
N1 C5 1.432(8) . ?
N1 C1 1.437(9) . ?
N2 C34 1.360(9) . ?
N2 C35 1.388(10) . ?
F1 C19 1.31(2) . ?
F1' C19 1.25(4) . ?
F2 C19 1.21(2) . ?
F2' C19 1.29(5) . ?
F3 C19 1.44(3) . ?
F3' C19 1.17(3) . ?
O1 C18 1.195(8) . ?
O2 C18 1.114(8) . ?
C1 C2 1.373(9) . ?
C2 C3 1.389(8) . ?
C3 C4 1.357(10) . ?
C4 C5 1.368(10) . ?
C6 C7 1.314(9) . ?
C6 C11 1.364(10) . ?
C7 C8 1.334(11) . ?
C8 C9 1.348(11) . ?
C9 C10 1.337(11) . ?
C10 C11 1.392(11) . ?
C12 C17 1.358(9) . ?
C12 C13 1.397(10) . ?
C13 C14 1.380(10) . ?
C14 C15 1.400(11) . ?
C15 C16 1.341(12) . ?
C16 C17 1.380(9) . ?
C18 C19 1.644(14) . ?
C20 C21 1.328(8) . ?
C20 C22 1.488(9) . ?
C22 C27 1.377(9) . ?
C22 C23 1.393(8) . ?
C23 C24 1.365(9) . ?
C24 C25 1.352(11) . ?
C25 C26 1.386(10) . ?
C26 C27 1.390(9) . ?
C28 C33 1.340(10) . ?
C28 C29 1.368(11) . ?
C29 C30 1.398(10) . ?
C30 C31 1.345(13) . ?
C31 C32 1.394(13) . ?
C32 C33 1.417(10) . ?
C34 C38 1.399(10) . ?
C35 C36 1.381(11) . ?
C36 C37 1.370(12) . ?
C37 C38 1.367(10) . ?
C39 C44 1.372(10) . ?
C39 C40 1.376(9) . ?
C40 C41 1.365(10) . ?
C41 C42 1.374(11) . ?
C42 C43 1.367(11) . ?
C43 C44 1.381(10) . ?
