#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:09:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179364 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/61/4326171.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_4326171
loop_
_publ_author_name
'Luciano Cuesta'
'Dune Prat'
'Tatiana Soler'
'Rafael Navarro'
'Esteban P. Urriolabeitia'
_publ_contact_author_address
;
ICMA, CSIC-Universidad de Zaragoza, Plaza S. Francisco, 
50009 Zaragoza (Spain)
;
_publ_contact_author_email       esteban@unizar.es
_publ_contact_author_fax         (+34)976761187
_publ_contact_author_name        'Esteban P. Urriolabeitia'
_publ_contact_author_phone       (+34)976762302
_publ_section_title
;
 Novel Cyclopalladated Imino-thiophenes: Synthesis and Reactivity Toward
 Alkynes and Carbon Monoxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8598
_journal_page_last               8607
_journal_paper_doi               10.1021/ic201158v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C30 H20 Cl2 N2 Pd2 S2'
_chemical_formula_sum            'C30 H20 Cl2 N2 Pd2 S2'
_chemical_formula_weight         756.30
_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
_cell_angle_alpha                108.826(4)
_cell_angle_beta                 100.350(4)
_cell_angle_gamma                101.074(4)
_cell_formula_units_Z            1
_cell_length_a                   6.1334(11)
_cell_length_b                   10.3097(18)
_cell_length_c                   11.480(2)
_cell_measurement_reflns_used    1157
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      22.8
_cell_measurement_theta_min      2.3
_cell_volume                     651.1(2)
_computing_cell_refinement       'Bruker SMART V5.625'
_computing_data_collection       'Bruker SMART V5.625'
_computing_data_reduction        'Bruker SAINT V6.28A'
_computing_molecular_graphics    'SHELXTL  Rel. 6.12/V (Siemens, 1996)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6342
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.772
_exptl_absorpt_correction_T_max  0.9652
_exptl_absorpt_correction_T_min  0.8780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker/Siemens SADABS V2.03'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_description       plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0409
_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)+(0.0358P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                2400
_reflns_number_total             2986
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic201158v_si_002_2.cif
_cod_data_source_block           '__2b'
_cod_database_code               4326171
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
Pd1 Pd 0.75440(6) 0.10515(4) 0.50249(3) 0.02228(12) Uani 1 1 d .
Cl1 Cl 0.61842(18) 0.02237(13) 0.64903(11) 0.0283(3) Uani 1 1 d .
C1 C 1.0567(7) 0.2089(5) 0.6179(4) 0.0241(10) Uani 1 1 d .
S1 S 1.1755(2) 0.24684(14) 0.77740(11) 0.0295(3) Uani 1 1 d .
C2 C 1.4384(8) 0.3505(5) 0.7755(5) 0.0265(10) Uani 1 1 d .
C3 C 1.6301(8) 0.4253(5) 0.8765(5) 0.0327(12) Uani 1 1 d .
H3 H 1.6300 0.4253 0.9575 0.039 Uiso 1 1 calc R
C4 C 1.8202(8) 0.4994(5) 0.8561(5) 0.0344(12) Uani 1 1 d .
H4 H 1.9495 0.5509 0.9238 0.041 Uiso 1 1 calc R
C5 C 1.8214(8) 0.4982(5) 0.7339(5) 0.0341(12) Uani 1 1 d .
H5 H 1.9533 0.5474 0.7213 0.041 Uiso 1 1 calc R
C6 C 1.6320(8) 0.4261(5) 0.6325(5) 0.0293(11) Uani 1 1 d .
H6 H 1.6352 0.4260 0.5518 0.035 Uiso 1 1 calc R
C7 C 1.4318(7) 0.3518(5) 0.6525(5) 0.0247(10) Uani 1 1 d .
C8 C 1.2121(8) 0.2711(5) 0.5649(4) 0.0240(10) Uani 1 1 d .
C9 C 1.1204(8) 0.2538(5) 0.4371(4) 0.0242(10) Uani 1 1 d .
H9 H 1.2106 0.2899 0.3918 0.029 Uiso 1 1 calc R
N1 N 0.9053(6) 0.1856(4) 0.3857(3) 0.0247(8) Uani 1 1 d .
C10 C 0.8059(7) 0.1733(5) 0.2580(4) 0.0240(10) Uani 1 1 d .
C11 C 0.6078(8) 0.2153(5) 0.2336(5) 0.0293(11) Uani 1 1 d .
H11 H 0.5322 0.2436 0.2969 0.035 Uiso 1 1 calc R
C12 C 0.5232(8) 0.2146(5) 0.1128(5) 0.0363(12) Uani 1 1 d .
H12 H 0.3912 0.2443 0.0957 0.044 Uiso 1 1 calc R
C13 C 0.6323(9) 0.1702(5) 0.0173(5) 0.0329(12) Uani 1 1 d .
H13 H 0.5727 0.1686 -0.0637 0.039 Uiso 1 1 calc R
C14 C 0.8286(8) 0.1286(5) 0.0431(5) 0.0300(11) Uani 1 1 d .
H14 H 0.9032 0.0995 -0.0206 0.036 Uiso 1 1 calc R
C15 C 0.9171(8) 0.1292(5) 0.1630(4) 0.0291(11) Uani 1 1 d .
H15 H 1.0501 0.1004 0.1798 0.035 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'
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_3
C1 Pd1 N1 80.26(17) .
C1 Pd1 Cl1 94.20(13) .
N1 Pd1 Cl1 174.41(11) .
C1 Pd1 Cl1 177.63(14) 2_656
N1 Pd1 Cl1 97.39(11) 2_656
Cl1 Pd1 Cl1 88.15(4) 2_656
Pd1 Cl1 Pd1 91.85(4) 2_656
C8 C1 S1 111.2(3) .
C8 C1 Pd1 114.9(3) .
S1 C1 Pd1 133.8(3) .
C1 S1 C2 92.4(2) .
C3 C2 C7 121.6(4) .
C3 C2 S1 127.7(4) .
C7 C2 S1 110.7(3) .
C4 C3 C2 119.2(5) .
C4 C3 H3 120.4 .
C2 C3 H3 120.4 .
C3 C4 C5 120.4(5) .
C3 C4 H4 119.8 .
C5 C4 H4 119.8 .
C6 C5 C4 121.4(5) .
C6 C5 H5 119.3 .
C4 C5 H5 119.3 .
C5 C6 C7 119.0(5) .
C5 C6 H6 120.5 .
C7 C6 H6 120.5 .
C2 C7 C6 118.4(4) .
C2 C7 C8 111.3(4) .
C6 C7 C8 130.3(4) .
C1 C8 C9 114.2(4) .
C1 C8 C7 114.3(4) .
C9 C8 C7 131.2(4) .
N1 C9 C8 117.2(4) .
N1 C9 H9 121.4 .
C8 C9 H9 121.4 .
C9 N1 C10 118.0(4) .
C9 N1 Pd1 113.2(3) .
C10 N1 Pd1 128.9(3) .
C11 C10 C15 120.6(4) .
C11 C10 N1 119.0(4) .
C15 C10 N1 120.2(4) .
C10 C11 C12 118.8(5) .
C10 C11 H11 120.6 .
C12 C11 H11 120.6 .
C13 C12 C11 121.0(5) .
C13 C12 H12 119.5 .
C11 C12 H12 119.5 .
C14 C13 C12 119.5(5) .
C14 C13 H13 120.3 .
C12 C13 H13 120.3 .
C13 C14 C15 120.6(5) .
C13 C14 H14 119.7 .
C15 C14 H14 119.7 .
C14 C15 C10 119.5(5) .
C14 C15 H15 120.3 .
C10 C15 H15 120.3 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C1 1.944(4) .
Pd1 N1 2.051(4) .
Pd1 Cl1 2.3263(12) .
Pd1 Cl1 2.4337(12) 2_656
Cl1 Pd1 2.4337(12) 2_656
C1 C8 1.384(6) .
C1 S1 1.728(5) .
S1 C2 1.763(5) .
C2 C3 1.381(7) .
C2 C7 1.410(6) .
C3 C4 1.367(7) .
C3 H3 0.9300 .
C4 C5 1.400(7) .
C4 H4 0.9300 .
C5 C6 1.372(7) .
C5 H5 0.9300 .
C6 C7 1.415(6) .
C6 H6 0.9300 .
C7 C8 1.436(6) .
C8 C9 1.414(6) .
C9 N1 1.296(6) .
C9 H9 0.9300 .
N1 C10 1.438(5) .
C10 C11 1.378(6) .
C10 C15 1.389(6) .
C11 C12 1.388(7) .
C11 H11 0.9300 .
C12 C13 1.384(7) .
C12 H12 0.9300 .
C13 C14 1.369(7) .
C13 H13 0.9300 .
C14 C15 1.382(6) .
C14 H14 0.9300 .
C15 H15 0.9300 .
