#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:50:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179866 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/62/7016258.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_7016258
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            'C34 H30 N2 Pd S2'
_chemical_formula_weight         637.12
_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                71.054(8)
_cell_angle_beta                 87.763(9)
_cell_angle_gamma                84.421(9)
_cell_formula_units_Z            2
_cell_length_a                   8.860(4)
_cell_length_b                   11.554(6)
_cell_length_c                   14.640(7)
_cell_measurement_reflns_used    1019
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      52.803
_cell_measurement_theta_min      5.680
_cell_volume                     1410.7(12)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12335
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.802996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (G.M.Sheldrick,SADABS,1996)
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0315
_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)+(0.0388P)²+0.5730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                4789
_reflns_number_total             5732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10598a.txt
_cod_data_source_block           7
_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        1410.6(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7016258
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 0.91317(2) 0.865147(19) 0.739436(15) 0.04578(9) Uani 1 1 d . . .
C7 C 1.0411(3) 0.7834(2) 0.6567(2) 0.0436(6) Uani 1 1 d . . .
N1 N 1.0407(3) 1.01113(19) 0.70095(16) 0.0445(5) Uani 1 1 d . . .
S1 S 0.73878(10) 0.72101(8) 0.78434(7) 0.0625(2) Uani 1 1 d . . .
S2 S 0.73291(10) 0.93332(8) 0.84320(6) 0.0598(2) Uani 1 1 d . . .
C1 C 1.1756(3) 0.9676(2) 0.5658(2) 0.0442(6) Uani 1 1 d . . .
C2 C 1.2731(3) 1.0218(3) 0.4911(2) 0.0535(7) Uani 1 1 d . . .
H2 H 1.2885 1.1041 0.4782 0.064 Uiso 1 1 calc R . .
C3 C 1.3476(3) 0.9589(3) 0.4356(2) 0.0528(7) Uani 1 1 d . . .
H3 H 1.4105 0.9997 0.3856 0.063 Uiso 1 1 calc R . .
C4 C 1.3311(3) 0.8360(2) 0.45245(19) 0.0431(6) Uani 1 1 d . . .
C5 C 1.2252(3) 0.7772(2) 0.52567(18) 0.0392(5) Uani 1 1 d . . .
C6 C 1.1446(3) 0.8424(2) 0.58352(19) 0.0407(6) Uani 1 1 d . . .
C8 C 1.0267(3) 0.6604(3) 0.6694(2) 0.0541(7) Uani 1 1 d . . .
H8 H 0.9624 0.6185 0.7181 0.065 Uiso 1 1 calc R . .
C9 C 1.1028(3) 0.5973(2) 0.6138(2) 0.0519(7) Uani 1 1 d . . .
H9 H 1.0882 0.5149 0.6264 0.062 Uiso 1 1 calc R . .
C10 C 1.1997(3) 0.6522(2) 0.5401(2) 0.0433(6) Uani 1 1 d . . .
C11 C 1.2736(3) 0.5875(2) 0.4773(2) 0.0434(6) Uani 1 1 d . . .
C12 C 1.3852(3) 0.6438(2) 0.4098(2) 0.0450(6) Uani 1 1 d . . .
C13 C 1.4188(3) 0.7658(3) 0.39806(19) 0.0456(6) Uani 1 1 d . . .
C14 C 1.5339(3) 0.8141(3) 0.3342(2) 0.0576(8) Uani 1 1 d . . .
H14 H 1.5575 0.8935 0.3263 0.069 Uiso 1 1 calc R . .
C15 C 1.6149(4) 0.7479(3) 0.2817(2) 0.0658(9) Uani 1 1 d . . .
H15 H 1.6932 0.7822 0.2408 0.079 Uiso 1 1 calc R . .
C16 C 1.5800(4) 0.6328(3) 0.2902(2) 0.0626(8) Uani 1 1 d . . .
H16 H 1.6339 0.5895 0.2540 0.075 Uiso 1 1 calc R . .
C17 C 1.4642(3) 0.5786(3) 0.3524(2) 0.0515(7) Uani 1 1 d . . .
C18 C 1.4236(4) 0.4602(3) 0.3606(2) 0.0595(8) Uani 1 1 d . . .
H18 H 1.4743 0.4165 0.3236 0.071 Uiso 1 1 calc R . .
C19 C 1.3115(4) 0.4101(3) 0.4220(2) 0.0596(8) Uani 1 1 d . . .
H19 H 1.2837 0.3333 0.4252 0.072 Uiso 1 1 calc R . .
C20 C 1.2372(3) 0.4721(3) 0.4803(2) 0.0526(7) Uani 1 1 d . . .
H20 H 1.1613 0.4353 0.5223 0.063 Uiso 1 1 calc R . .
C21 C 1.1233(3) 1.0417(2) 0.6244(2) 0.0479(6) Uani 1 1 d . . .
H21 H 1.1528 1.1213 0.6047 0.057 Uiso 1 1 calc R . .
C22 C 1.0171(3) 1.0968(2) 0.7541(2) 0.0438(6) Uani 1 1 d . . .
C23 C 1.0571(4) 1.0576(3) 0.8501(2) 0.0543(7) Uani 1 1 d . . .
H23 H 1.0950 0.9766 0.8800 0.065 Uiso 1 1 calc R . .
C24 C 1.0405(4) 1.1394(3) 0.9019(2) 0.0614(8) Uani 1 1 d . . .
H24 H 1.0724 1.1135 0.9657 0.074 Uiso 1 1 calc R . .
C25 C 0.9778(4) 1.2583(3) 0.8608(2) 0.0571(8) Uani 1 1 d . . .
C26 C 0.9353(4) 1.2950(3) 0.7655(2) 0.0594(8) Uani 1 1 d . . .
H26 H 0.8923 1.3748 0.7365 0.071 Uiso 1 1 calc R . .
C27 C 0.9554(3) 1.2155(3) 0.7118(2) 0.0537(7) Uani 1 1 d . . .
H27 H 0.9272 1.2423 0.6473 0.064 Uiso 1 1 calc R . .
C28 C 0.9626(5) 1.3464(4) 0.9192(3) 0.0816(11) Uani 1 1 d . . .
H28A H 0.8872 1.4137 0.8895 0.098 Uiso 1 1 calc R . .
H28B H 0.9273 1.3037 0.9839 0.098 Uiso 1 1 calc R . .
C29 C 1.1085(6) 1.3970(4) 0.9255(4) 0.1049(15) Uani 1 1 d . . .
H29A H 1.1823 1.3310 0.9573 0.157 Uiso 1 1 calc R . .
H29B H 1.0934 1.4532 0.9617 0.157 Uiso 1 1 calc R . .
H29C H 1.1439 1.4393 0.8617 0.157 Uiso 1 1 calc R . .
C31 C 0.6436(3) 0.8068(3) 0.8484(2) 0.0554(7) Uani 1 1 d . . .
N2 N 0.5155(3) 0.7769(3) 0.8958(2) 0.0690(8) Uani 1 1 d . . .
C32 C 0.4322(5) 0.8542(4) 0.9476(3) 0.0867(12) Uani 1 1 d . . .
H32A H 0.4605 0.9376 0.9206 0.104 Uiso 1 1 calc R . .
H32B H 0.3242 0.8558 0.9380 0.104 Uiso 1 1 calc R . .
C33 C 0.4638(7) 0.8088(6) 1.0522(4) 0.128(2) Uani 1 1 d . . .
H33A H 0.4417 0.7245 1.0786 0.193 Uiso 1 1 calc R . .
H33B H 0.4016 0.8575 1.0837 0.193 Uiso 1 1 calc R . .
H33C H 0.5688 0.8148 1.0624 0.193 Uiso 1 1 calc R . .
C34 C 0.4427(4) 0.6656(4) 0.8950(3) 0.0852(12) Uani 1 1 d . . .
H34A H 0.5194 0.6044 0.8858 0.102 Uiso 1 1 calc R . .
H34B H 0.3919 0.6301 0.9563 0.102 Uiso 1 1 calc R . .
C35 C 0.3325(6) 0.7011(6) 0.8163(4) 0.1221(19) Uani 1 1 d . . .
H35A H 0.2495 0.7527 0.8303 0.183 Uiso 1 1 calc R . .
H35B H 0.2951 0.6287 0.8101 0.183 Uiso 1 1 calc R . .
H35C H 0.3807 0.7450 0.7569 0.183 Uiso 1 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'
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
C7 Pd1 N1 91.63(10) . . ?
C7 Pd1 S1 95.69(8) . . ?
N1 Pd1 S1 171.34(7) . . ?
C7 Pd1 S2 169.93(8) . . ?
N1 Pd1 S2 98.40(7) . . ?
S1 Pd1 S2 74.24(4) . . ?
C8 C7 C6 116.2(2) . . ?
C8 C7 Pd1 118.6(2) . . ?
C6 C7 Pd1 125.18(19) . . ?
C21 N1 C22 117.4(2) . . ?
C21 N1 Pd1 124.27(18) . . ?
C22 N1 Pd1 117.49(17) . . ?
C31 S1 Pd1 88.30(11) . . ?
C31 S2 Pd1 85.01(11) . . ?
C2 C1 C21 115.0(2) . . ?
C2 C1 C6 119.4(2) . . ?
C21 C1 C6 125.4(2) . . ?
C3 C2 C1 122.5(3) . . ?
C2 C3 C4 121.3(3) . . ?
C3 C4 C5 118.3(2) . . ?
C3 C4 C13 121.6(3) . . ?
C5 C4 C13 120.1(2) . . ?
C10 C5 C6 119.9(2) . . ?
C10 C5 C4 119.1(2) . . ?
C6 C5 C4 121.0(2) . . ?
C7 C6 C5 120.8(2) . . ?
C7 C6 C1 122.0(2) . . ?
C5 C6 C1 117.3(2) . . ?
C9 C8 C7 123.4(3) . . ?
C10 C9 C8 122.1(2) . . ?
C9 C10 C5 117.5(2) . . ?
C9 C10 C11 122.2(2) . . ?
C5 C10 C11 120.3(2) . . ?
C20 C11 C12 118.0(3) . . ?
C20 C11 C10 122.3(3) . . ?
C12 C11 C10 119.7(2) . . ?
C11 C12 C17 120.0(2) . . ?
C11 C12 C13 120.6(2) . . ?
C17 C12 C13 119.3(3) . . ?
C14 C13 C12 118.1(3) . . ?
C14 C13 C4 122.4(3) . . ?
C12 C13 C4 119.5(2) . . ?
C15 C14 C13 122.1(3) . . ?
C16 C15 C14 120.0(3) . . ?
C15 C16 C17 121.0(3) . . ?
C16 C17 C18 121.9(3) . . ?
C16 C17 C12 119.3(3) . . ?
C18 C17 C12 118.8(3) . . ?
C19 C18 C17 120.4(3) . . ?
C18 C19 C20 120.9(3) . . ?
C11 C20 C19 121.6(3) . . ?
N1 C21 C1 127.6(2) . . ?
C27 C22 C23 119.5(3) . . ?
C27 C22 N1 121.8(2) . . ?
C23 C22 N1 118.6(2) . . ?
C22 C23 C24 119.7(3) . . ?
C25 C24 C23 121.4(3) . . ?
C26 C25 C24 118.0(3) . . ?
C26 C25 C28 121.8(3) . . ?
C24 C25 C28 120.1(3) . . ?
C25 C26 C27 121.3(3) . . ?
C22 C27 C26 120.0(3) . . ?
C29 C28 C25 112.2(3) . . ?
N2 C31 S2 124.6(2) . . ?
N2 C31 S1 123.0(2) . . ?
S2 C31 S1 112.41(18) . . ?
C31 N2 C32 122.3(3) . . ?
C31 N2 C34 121.2(3) . . ?
C32 N2 C34 116.4(3) . . ?
C33 C32 N2 112.3(4) . . ?
C35 C34 N2 109.2(4) . . ?
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 C7 2.018(3) . ?
Pd1 N1 2.035(2) . ?
Pd1 S1 2.3027(11) . ?
Pd1 S2 2.4128(11) . ?
C7 C8 1.390(4) . ?
C7 C6 1.423(4) . ?
N1 C21 1.283(4) . ?
N1 C22 1.441(3) . ?
S1 C31 1.718(3) . ?
S2 C31 1.708(3) . ?
C1 C2 1.386(4) . ?
C1 C21 1.434(4) . ?
C1 C6 1.436(4) . ?
C2 C3 1.367(4) . ?
C3 C4 1.382(4) . ?
C4 C5 1.436(4) . ?
C4 C13 1.464(4) . ?
C5 C10 1.430(4) . ?
C5 C6 1.434(4) . ?
C8 C9 1.378(4) . ?
C9 C10 1.376(4) . ?
C10 C11 1.462(4) . ?
C11 C20 1.389(4) . ?
C11 C12 1.417(4) . ?
C12 C17 1.423(4) . ?
C12 C13 1.423(4) . ?
C13 C14 1.387(4) . ?
C14 C15 1.386(4) . ?
C15 C16 1.360(5) . ?
C16 C17 1.398(4) . ?
C17 C18 1.414(4) . ?
C18 C19 1.355(5) . ?
C19 C20 1.390(4) . ?
C22 C27 1.375(4) . ?
C22 C23 1.379(4) . ?
C23 C24 1.385(4) . ?
C24 C25 1.378(5) . ?
C25 C26 1.376(5) . ?
C25 C28 1.522(4) . ?
C26 C27 1.385(4) . ?
C28 C29 1.487(6) . ?
C31 N2 1.322(4) . ?
N2 C32 1.478(4) . ?
N2 C34 1.497(5) . ?
C32 C33 1.477(7) . ?
C34 C35 1.467(6) . ?
