#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:32:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179975 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/69/7026999.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7026999
loop_
_publ_author_name
'Falvello, Larry R.'
'Fernández, Susana'
'García, María M.'
'Navarro, Rafael'
'Urriolabeitia, Esteban P.'
_publ_section_title
;
 Synthesis and characterization of complexes of PdII and PtII containing
 the iminophosphorane ligand Ph3PNCN
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3745
_journal_paper_doi               10.1039/a805147j
_journal_year                    1998
_chemical_formula_sum            'C38 H30 Cl2 N4 P2 Pd'
_chemical_formula_weight         781.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.862(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5452(7)
_cell_length_b                   12.9923(5)
_cell_length_c                   13.8799(7)
_cell_measurement_temperature    150(2)
_cell_volume                     1717.39(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3226
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.85904
_exptl_absorpt_correction_T_min  0.69596
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_obs          0.0349
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0651P)²+0.4530P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1006
_refine_ls_wR_factor_obs         0.0937
_reflns_number_observed          2595
_reflns_number_total             3022
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            805147jsup1.cif
_cod_data_source_block           cad6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.4530P] 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^)+(0.0651P)^2^+0.4530P] 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        1717.4(2)
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               7026999
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.0000 0.0000 0.0000 0.02408(14) Uani 1 d S
P1 P 0.25747(8) -0.33841(6) 0.15828(6) 0.0228(2) Uani 1 d .
Cl1 Cl 0.18251(9) 0.10297(6) -0.04067(6) 0.0347(2) Uani 1 d .
N1 N 0.1276(3) -0.1183(2) 0.0215(2) 0.0327(6) Uani 1 d .
C1 C 0.1696(3) -0.1995(2) 0.0397(2) 0.0251(6) Uani 1 d .
N2 N 0.2182(3) -0.2917(2) 0.0525(2) 0.0266(6) Uani 1 d .
C2 C 0.3754(3) -0.2565(2) 0.2287(2) 0.0248(6) Uani 1 d .
C3 C 0.4891(3) -0.2171(2) 0.1820(2) 0.0314(7) Uani 1 d .
H3A H 0.4987(3) -0.2325(2) 0.1159(2) 0.038 Uiso 1 calc R
C4 C 0.5870(4) -0.1562(3) 0.2320(3) 0.0366(8) Uani 1 d .
H4A H 0.6636(4) -0.1286(3) 0.2001(3) 0.044 Uiso 1 calc R
C5 C 0.5738(4) -0.1354(3) 0.3282(3) 0.0377(8) Uani 1 d .
H5A H 0.6432(4) -0.0951(3) 0.3630(3) 0.045 Uiso 1 calc R
C6 C 0.4613(4) -0.1724(3) 0.3742(3) 0.0390(8) Uani 1 d .
H6A H 0.4517(4) -0.1562(3) 0.4402(3) 0.047 Uiso 1 calc R
C7 C 0.3617(4) -0.2334(3) 0.3244(2) 0.0333(7) Uani 1 d .
H7A H 0.2840(4) -0.2593(3) 0.3562(2) 0.040 Uiso 1 calc R
C8 C 0.3472(3) -0.4567(2) 0.1389(2) 0.0269(7) Uani 1 d .
C9 C 0.4450(4) -0.4949(2) 0.2087(3) 0.0359(8) Uani 1 d .
H9A H 0.4655(4) -0.4577(2) 0.2669(3) 0.043 Uiso 1 calc R
C10 C 0.5127(4) -0.5872(3) 0.1930(3) 0.0437(9) Uani 1 d .
H10A H 0.5793(4) -0.6135(3) 0.2407(3) 0.052 Uiso 1 calc R
C11 C 0.4836(4) -0.6406(3) 0.1090(3) 0.0464(10) Uani 1 d .
H11A H 0.5313(4) -0.7033(3) 0.0981(3) 0.056 Uiso 1 calc R
C12 C 0.3849(4) -0.6037(3) 0.0397(3) 0.0456(9) Uani 1 d .
H12A H 0.3636(4) -0.6417(3) -0.0179(3) 0.055 Uiso 1 calc R
C13 C 0.3176(4) -0.5117(3) 0.0546(3) 0.0358(8) Uani 1 d .
H13A H 0.2507(4) -0.4860(3) 0.0068(3) 0.043 Uiso 1 calc R
C14 C 0.1044(3) -0.3650(2) 0.2225(2) 0.0257(6) Uani 1 d .
C15 C -0.0264(3) -0.3315(2) 0.1854(2) 0.0311(7) Uani 1 d .
H15A H -0.0344(3) -0.2948(2) 0.1261(2) 0.037 Uiso 1 calc R
C16 C -0.1454(4) -0.3514(3) 0.2345(3) 0.0391(8) Uani 1 d .
H16A H -0.2352(4) -0.3306(3) 0.2079(3) 0.047 Uiso 1 calc R
C17 C -0.1325(4) -0.4014(3) 0.3221(3) 0.0467(10) Uani 1 d .
H17A H -0.2134(4) -0.4134(3) 0.3568(3) 0.056 Uiso 1 calc R
C18 C -0.0023(4) -0.4343(3) 0.3601(3) 0.0459(10) Uani 1 d .
H18A H 0.0055(4) -0.4685(3) 0.4207(3) 0.055 Uiso 1 calc R
C19 C 0.1157(4) -0.4177(3) 0.3106(2) 0.0370(8) Uani 1 d .
H19A H 0.2045(4) -0.4418(3) 0.3362(2) 0.044 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 N1 180.0 3 . y
N1 Pd1 Cl1 88.84(9) 3 . y
N1 Pd1 Cl1 91.16(9) . . y
N1 Pd1 Cl1 91.16(9) 3 3 ?
N1 Pd1 Cl1 88.84(9) . 3 ?
Cl1 Pd1 Cl1 180.0 . 3 ?
N2 P1 C8 105.74(14) . . y
N2 P1 C2 111.91(14) . . y
C8 P1 C2 107.65(14) . . y
N2 P1 C14 112.23(14) . . y
C8 P1 C14 108.84(14) . . y
C2 P1 C14 110.22(14) . . y
C1 N1 Pd1 161.9(3) . . y
N1 C1 N2 175.2(3) . . y
C1 N2 P1 122.3(2) . . y
C7 C2 C3 119.7(3) . . ?
C7 C2 P1 124.0(2) . . ?
C3 C2 P1 116.3(2) . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3A 120.1(2) . . ?
C2 C3 H3A 120.1(2) . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4A 120.0(2) . . ?
C5 C4 H4A 120.0(2) . . ?
C6 C5 C4 120.6(3) . . ?
C6 C5 H5A 119.7(2) . . ?
C4 C5 H5A 119.7(2) . . ?
C5 C6 C7 119.9(3) . . ?
C5 C6 H6A 120.0(2) . . ?
C7 C6 H6A 120.0(2) . . ?
C2 C7 C6 120.0(3) . . ?
C2 C7 H7A 120.0(2) . . ?
C6 C7 H7A 120.0(2) . . ?
C13 C8 C9 119.6(3) . . ?
C13 C8 P1 119.9(2) . . ?
C9 C8 P1 120.5(3) . . ?
C10 C9 C8 119.8(4) . . ?
C10 C9 H9A 120.1(2) . . ?
C8 C9 H9A 120.1(2) . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H10A 119.9(2) . . ?
C9 C10 H10A 119.9(2) . . ?
C10 C11 C12 120.3(3) . . ?
C10 C11 H11A 119.8(2) . . ?
C12 C11 H11A 119.8(2) . . ?
C13 C12 C11 119.9(4) . . ?
C13 C12 H12A 120.1(2) . . ?
C11 C12 H12A 120.1(2) . . ?
C12 C13 C8 120.2(3) . . ?
C12 C13 H13A 119.9(2) . . ?
C8 C13 H13A 119.9(2) . . ?
C15 C14 C19 119.5(3) . . ?
C15 C14 P1 119.8(2) . . ?
C19 C14 P1 120.7(2) . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15A 119.8(2) . . ?
C16 C15 H15A 119.8(2) . . ?
C17 C16 C15 119.6(4) . . ?
C17 C16 H16A 120.2(2) . . ?
C15 C16 H16A 120.2(2) . . ?
C16 C17 C18 120.4(4) . . ?
C16 C17 H17A 119.8(2) . . ?
C18 C17 H17A 119.8(2) . . ?
C19 C18 C17 120.4(4) . . ?
C19 C18 H18A 119.8(2) . . ?
C17 C18 H18A 119.8(2) . . ?
C18 C19 C14 119.7(3) . . ?
C18 C19 H19A 120.2(2) . . ?
C14 C19 H19A 120.2(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 N1 1.971(3) 3 ?
Pd1 N1 1.971(3) . y
Pd1 Cl1 2.2969(9) . y
Pd1 Cl1 2.2969(9) 3 ?
P1 N2 1.609(3) . y
P1 C8 1.789(3) . y
P1 C2 1.791(3) . y
P1 C14 1.796(3) . y
N1 C1 1.151(4) . y
C1 N2 1.292(4) . y
C2 C7 1.375(5) . ?
C2 C3 1.398(4) . ?
C3 C4 1.377(5) . ?
C3 H3A 0.95 . ?
C4 C5 1.376(5) . ?
C4 H4A 0.95 . ?
C5 C6 1.373(5) . ?
C5 H5A 0.95 . ?
C6 C7 1.387(5) . ?
C6 H6A 0.95 . ?
C7 H7A 0.95 . ?
C8 C13 1.384(5) . ?
C8 C9 1.391(4) . ?
C9 C10 1.386(5) . ?
C9 H9A 0.95 . ?
C10 C11 1.370(6) . ?
C10 H10A 0.95 . ?
C11 C12 1.385(5) . ?
C11 H11A 0.95 . ?
C12 C13 1.380(5) . ?
C12 H12A 0.95 . ?
C13 H13A 0.95 . ?
C14 C15 1.388(4) . ?
C14 C19 1.399(5) . ?
C15 C16 1.388(5) . ?
C15 H15A 0.95 . ?
C16 C17 1.377(6) . ?
C16 H16A 0.95 . ?
C17 C18 1.384(6) . ?
C17 H17A 0.95 . ?
C18 C19 1.375(5) . ?
C18 H18A 0.95 . ?
C19 H19A 0.95 . ?
