#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:50:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179866 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/62/7016259.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_7016259
loop_
_publ_author_name
'Lentijo, Sergio'
'Miguel, Jesús A'
'Espinet, Pablo'
_publ_section_title
;
 Cyclopalladated complexes of perylene imine: mononuclear complexes
 with five- or six-membered metallacycles.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7602
_journal_page_last               7609
_journal_paper_doi               10.1039/c1dt10598a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C31 H23 N O Pd S2'
_chemical_formula_weight         596.02
_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-97
_cell_angle_alpha                94.315(6)
_cell_angle_beta                 103.724(6)
_cell_angle_gamma                106.064(6)
_cell_formula_units_Z            2
_cell_length_a                   7.834(3)
_cell_length_b                   10.954(4)
_cell_length_c                   15.586(5)
_cell_measurement_reflns_used    743
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.828
_cell_measurement_theta_min      5.094
_cell_volume                     1234.3(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10784
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.705834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (G.M.Sheldrick,SADABS,1996)
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0450
_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)+(0.0599P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                3183
_reflns_number_total             5044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10598a.txt
_cod_data_source_block           8
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1234.3(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7016259
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.18405(6) 0.13996(4) 0.24094(3) 0.04209(16) Uani 1 1 d . . .
S2 S 0.3404(2) 0.08728(15) 0.38005(10) 0.0585(4) Uani 1 1 d . . .
S1 S 0.4691(2) 0.29275(15) 0.28586(10) 0.0586(4) Uani 1 1 d . . .
N1 N -0.0667(6) 0.0008(4) 0.2004(3) 0.0399(10) Uani 1 1 d . . .
C2 C 0.0864(7) 0.1892(5) 0.1223(3) 0.0426(13) Uani 1 1 d . . .
C1 C -0.0783(7) 0.0996(5) 0.0721(3) 0.0388(12) Uani 1 1 d . . .
C21 C -0.1547(7) -0.0029(5) 0.1186(4) 0.0406(12) Uani 1 1 d . . .
H21 H -0.2628 -0.0685 0.0906 0.049 Uiso 1 1 calc R . .
C3 C 0.1636(7) 0.2964(5) 0.0856(3) 0.0436(13) Uani 1 1 d . . .
H3 H 0.2756 0.3547 0.1181 0.052 Uiso 1 1 calc R . .
C4 C 0.0780(7) 0.3188(5) 0.0017(3) 0.0374(12) Uani 1 1 d . . .
C5 C -0.0861(7) 0.2269(5) -0.0510(3) 0.0384(12) Uani 1 1 d . . .
C6 C -0.1657(7) 0.1139(5) -0.0164(3) 0.0401(12) Uani 1 1 d . . .
C7 C -0.3262(8) 0.0238(5) -0.0695(4) 0.0487(14) Uani 1 1 d . . .
H7 H -0.3779 -0.0503 -0.0476 0.058 Uiso 1 1 calc R . .
C8 C -0.4100(8) 0.0419(6) -0.1534(4) 0.0514(14) Uani 1 1 d . . .
H8 H -0.5169 -0.0196 -0.1880 0.062 Uiso 1 1 calc R . .
C9 C -0.3340(8) 0.1522(6) -0.1860(4) 0.0486(14) Uani 1 1 d . . .
H9 H -0.3924 0.1643 -0.2426 0.058 Uiso 1 1 calc R . .
C10 C -0.1739(7) 0.2450(5) -0.1373(3) 0.0404(12) Uani 1 1 d . . .
C11 C -0.0956(8) 0.3634(5) -0.1720(3) 0.0454(14) Uani 1 1 d . . .
C12 C 0.0671(7) 0.4555(5) -0.1198(3) 0.0404(13) Uani 1 1 d . . .
C13 C 0.1574(7) 0.4380(5) -0.0324(3) 0.0386(12) Uani 1 1 d . . .
C14 C 0.3119(8) 0.5325(5) 0.0161(4) 0.0458(13) Uani 1 1 d . . .
H14 H 0.3684 0.5233 0.0738 0.055 Uiso 1 1 calc R . .
C15 C 0.3880(8) 0.6431(5) -0.0186(4) 0.0519(15) Uani 1 1 d . . .
H15 H 0.4949 0.7049 0.0158 0.062 Uiso 1 1 calc R . .
C16 C 0.3068(8) 0.6604(5) -0.1017(4) 0.0516(15) Uani 1 1 d . . .
H16 H 0.3582 0.7343 -0.1239 0.062 Uiso 1 1 calc R . .
C17 C 0.1473(8) 0.5689(6) -0.1543(4) 0.0477(14) Uani 1 1 d . . .
C18 C 0.0574(9) 0.5856(7) -0.2399(4) 0.0640(18) Uani 1 1 d . . .
H18 H 0.1089 0.6579 -0.2637 0.077 Uiso 1 1 calc R . .
C19 C -0.1018(10) 0.4993(8) -0.2884(4) 0.079(2) Uani 1 1 d . . .
H19 H -0.1611 0.5140 -0.3441 0.095 Uiso 1 1 calc R . .
C20 C -0.1777(9) 0.3884(7) -0.2556(4) 0.0695(19) Uani 1 1 d . . .
H20 H -0.2865 0.3290 -0.2905 0.083 Uiso 1 1 calc R . .
C22 C -0.1404(7) -0.0920(5) 0.2515(3) 0.0384(12) Uani 1 1 d . . .
C23 C -0.1327(8) -0.0502(5) 0.3391(4) 0.0504(14) Uani 1 1 d . . .
H23 H -0.0793 0.0363 0.3630 0.060 Uiso 1 1 calc R . .
C24 C -0.2041(8) -0.1368(6) 0.3903(4) 0.0573(16) Uani 1 1 d . . .
H24 H -0.1997 -0.1074 0.4486 0.069 Uiso 1 1 calc R . .
C25 C -0.2830(8) -0.2672(5) 0.3577(4) 0.0455(13) Uani 1 1 d . . .
C26 C -0.2834(8) -0.3069(5) 0.2716(4) 0.0518(15) Uani 1 1 d . . .
H26 H -0.3316 -0.3940 0.2486 0.062 Uiso 1 1 calc R . .
C27 C -0.2145(7) -0.2215(5) 0.2186(4) 0.0434(13) Uani 1 1 d . . .
H27 H -0.2178 -0.2511 0.1605 0.052 Uiso 1 1 calc R . .
C28 C -0.3568(10) -0.3611(6) 0.4160(4) 0.0711(19) Uani 1 1 d . . .
H28A H -0.4144 -0.3207 0.4536 0.085 Uiso 1 1 calc R . .
H28B H -0.4512 -0.4351 0.3782 0.085 Uiso 1 1 calc R . .
C29 C -0.2162(13) -0.4049(9) 0.4725(6) 0.131(4) Uani 1 1 d . . .
H29A H -0.1485 -0.4359 0.4366 0.197 Uiso 1 1 calc R . .
H29B H -0.2738 -0.4730 0.5013 0.197 Uiso 1 1 calc R . .
H29C H -0.1333 -0.3348 0.5170 0.197 Uiso 1 1 calc R . .
C31 C 0.5136(8) 0.2140(6) 0.3732(4) 0.0520(14) Uani 1 1 d . . .
C32 C 0.7166(10) 0.1863(7) 0.5042(5) 0.091(2) Uani 1 1 d . . .
H32A H 0.6255 0.1804 0.5367 0.136 Uiso 1 1 calc R . .
H32B H 0.8366 0.2310 0.5431 0.136 Uiso 1 1 calc R . .
H32C H 0.7136 0.1014 0.4818 0.136 Uiso 1 1 calc R . .
O1 O 0.6777(6) 0.2551(4) 0.4307(3) 0.0763(13) 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
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C2 Pd1 N1 80.77(19) . . ?
C2 Pd1 S1 99.61(16) . . ?
N1 Pd1 S1 178.64(13) . . ?
C2 Pd1 S2 172.58(16) . . ?
N1 Pd1 S2 104.96(12) . . ?
S1 Pd1 S2 74.56(6) . . ?
C31 S2 Pd1 82.6(2) . . ?
C31 S1 Pd1 86.4(2) . . ?
C21 N1 C22 120.0(4) . . ?
C21 N1 Pd1 113.8(3) . . ?
C22 N1 Pd1 126.1(3) . . ?
C3 C2 C1 118.9(5) . . ?
C3 C2 Pd1 128.4(4) . . ?
C1 C2 Pd1 112.7(4) . . ?
C2 C1 C6 121.4(4) . . ?
C2 C1 C21 114.6(5) . . ?
C6 C1 C21 123.9(5) . . ?
N1 C21 C1 117.2(5) . . ?
C2 C3 C4 122.0(5) . . ?
C3 C4 C5 119.7(5) . . ?
C3 C4 C13 120.5(5) . . ?
C5 C4 C13 119.9(4) . . ?
C10 C5 C4 121.2(5) . . ?
C10 C5 C6 119.2(5) . . ?
C4 C5 C6 119.6(4) . . ?
C7 C6 C1 122.8(5) . . ?
C7 C6 C5 118.8(5) . . ?
C1 C6 C5 118.3(5) . . ?
C8 C7 C6 121.5(5) . . ?
C7 C8 C9 119.4(5) . . ?
C10 C9 C8 122.1(5) . . ?
C9 C10 C5 118.9(5) . . ?
C9 C10 C11 121.7(5) . . ?
C5 C10 C11 119.4(5) . . ?
C20 C11 C12 118.0(5) . . ?
C20 C11 C10 122.2(5) . . ?
C12 C11 C10 119.7(4) . . ?
C11 C12 C13 121.3(5) . . ?
C11 C12 C17 120.0(5) . . ?
C13 C12 C17 118.7(5) . . ?
C14 C13 C12 118.6(5) . . ?
C14 C13 C4 122.9(5) . . ?
C12 C13 C4 118.5(5) . . ?
C13 C14 C15 122.0(5) . . ?
C16 C15 C14 120.4(6) . . ?
C15 C16 C17 120.8(5) . . ?
C16 C17 C18 122.1(5) . . ?
C16 C17 C12 119.6(5) . . ?
C18 C17 C12 118.3(6) . . ?
C19 C18 C17 121.5(6) . . ?
C18 C19 C20 120.2(6) . . ?
C19 C20 C11 121.9(6) . . ?
C27 C22 C23 119.0(5) . . ?
C27 C22 N1 122.8(5) . . ?
C23 C22 N1 118.2(5) . . ?
C24 C23 C22 119.9(5) . . ?
C23 C24 C25 122.0(5) . . ?
C26 C25 C24 117.1(5) . . ?
C26 C25 C28 121.9(5) . . ?
C24 C25 C28 121.0(5) . . ?
C27 C26 C25 121.9(5) . . ?
C26 C27 C22 120.2(5) . . ?
C29 C28 C25 113.6(6) . . ?
O1 C31 S2 124.9(4) . . ?
O1 C31 S1 118.7(4) . . ?
S2 C31 S1 116.4(3) . . ?
C31 O1 C32 118.7(5) . . ?
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 C2 2.001(5) . ?
Pd1 N1 2.047(4) . ?
Pd1 S1 2.3003(17) . ?
Pd1 S2 2.4193(16) . ?
S2 C31 1.682(6) . ?
S1 C31 1.684(6) . ?
N1 C21 1.288(6) . ?
N1 C22 1.420(6) . ?
C2 C3 1.393(7) . ?
C2 C1 1.394(7) . ?
C1 C6 1.428(7) . ?
C1 C21 1.449(7) . ?
C3 C4 1.395(7) . ?
C4 C5 1.414(7) . ?
C4 C13 1.479(7) . ?
C5 C10 1.413(7) . ?
C5 C6 1.430(7) . ?
C6 C7 1.391(7) . ?
C7 C8 1.373(7) . ?
C8 C9 1.383(8) . ?
C9 C10 1.382(8) . ?
C10 C11 1.475(7) . ?
C11 C20 1.393(7) . ?
C11 C12 1.406(8) . ?
C12 C13 1.432(7) . ?
C12 C17 1.434(7) . ?
C13 C14 1.365(7) . ?
C14 C15 1.402(7) . ?
C15 C16 1.354(8) . ?
C16 C17 1.391(8) . ?
C17 C18 1.404(8) . ?
C18 C19 1.347(9) . ?
C19 C20 1.389(9) . ?
C22 C27 1.380(7) . ?
C22 C23 1.389(7) . ?
C23 C24 1.372(7) . ?
C24 C25 1.391(7) . ?
C25 C26 1.379(8) . ?
C25 C28 1.510(7) . ?
C26 C27 1.378(7) . ?
C28 C29 1.454(10) . ?
C31 O1 1.315(7) . ?
C32 O1 1.437(7) . ?
