#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:40:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178576 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/86/4068660.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_4068660
loop_
_publ_author_name
'Kaur, Rupinder'
'Menon, Saija C.'
'Panda, Snigdha'
'Singh, Harkesh B.'
'Patel, Rajan P.'
'Butcher, Ray J.'
_publ_section_title
;
 Facile Cleavage of Organochalcogen Hybrid (NEEN, NEN, EN, where E = Se or
 Te) Ligand C−E and E−E Bonds by Pd(II)
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2363
_journal_paper_doi               10.1021/om801015e
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C19 H26 Cl4 N2 Pd2 Te2'
_chemical_formula_weight         892.22
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.681(2)
_cell_length_b                   14.681(2)
_cell_length_c                   12.538(4)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.456
_cell_measurement_theta_min      3.157
_cell_volume                     2702.3(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/ω 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  0.0444
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5238
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         2.14
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.852
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.512
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         4894
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                4924
_reflns_number_total             4924
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om801015e_si_001.cif
_cod_data_source_block           29
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -42(1)c'
_cod_database_code               4068660
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'0.5-x, 0.5+y, 0.5-z'
'0.5+x, 0.5-y, 0.5-z'
'0.5-Y, 0.5-x, 0.5+z'
'0.5+y, 0.5+x, 0.5+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
Pd1 PD -0.1239(1) 0.0395(1) 0.1522(1) 0.045(1) Uani 1 1 d
Te1 TE 0.0334(1) 0.1070(1) 0.1277(1) 0.043(1) Uani 1 1 d
Cl1 CL -0.2567(1) -0.0463(1) 0.1865(2) 0.086(1) Uani 1 1 d
N1 N -0.1859(3) 0.1759(3) 0.1770(4) 0.050(1) Uani 1 1 d
C1 C 0.0125(4) 0.1611(4) 0.2836(5) 0.045(1) Uani 1 1 d
C2 C -0.0571(4) 0.2244(4) 0.2968(6) 0.047(1) Uani 1 1 d
C3 C -0.0703(5) 0.2639(4) 0.3943(6) 0.056(2) Uani 1 1 d
C4 C -0.0180(5) 0.2374(5) 0.4794(7) 0.075(2) Uani 1 1 d
C5 C 0.0489(5) 0.1717(5) 0.4697(6) 0.066(2) Uani 1 1 d
C6 C 0.0656(4) 0.1338(4) 0.3707(6) 0.059(2) Uani 1 1 d
C7 C -0.1173(5) 0.2474(4) 0.2034(6) 0.059(2) Uani 1 1 d
C8 C -0.2567(5) 0.1720(5) 0.2594(7) 0.067(2) Uani 1 1 d
C9 C -0.2291(5) 0.2029(5) 0.0737(7) 0.075(2) Uani 1 1 d
Cl1D CL -0.4102(3) -0.0063(4) -0.0245(4) 0.083(1) Uani 1 1 d
Cl2D CL -0.5049(5) 0.0365(5) -0.2218(6) 0.083(1) Uani 1 1 d
Cl3D CL -0.3988(5) 0.0431(5) -0.0557(5) 0.083(1) Uani 1 1 d
C1D C -0.5013(12) 0.0419(11) -0.1267(14) 0.080(4) Uani 1 1 d
H3A H -0.1167(5) 0.3061(4) 0.4044(6) 0.080 Uiso 1 1 d
H4A H -0.0256(5) 0.2663(5) 0.5448(7) 0.080 Uiso 1 1 d
H5A H 0.0821(5) 0.1531(5) 0.5290(6) 0.080 Uiso 1 1 d
H6A H 0.1115(4) 0.0907(4) 0.3629(6) 0.080 Uiso 1 1 d
H7A H -.0791(5) 0.2584(4) 0.1416(6) 0.080 Uiso 1 1 d
H7B H -0.1497(5) 0.3035(4) 0.2191(6) 0.080 Uiso 1 1 d
H8A H -0.2839(5) 0.2311(5) 0.2676(7) 0.080 Uiso 1 1 d
H8B H -0.2297(5) 0.1536(5) 0.3257(7) 0.080 Uiso 1 1 d
H8C H -0.3027(5) 0.1288(5) 0.2392(7) 0.080 Uiso 1 1 d
H9A H -0.2415(5) 0.2671(5) 0.0738(7) 0.080 Uiso 1 1 d
H9B H -0.2850(5) 0.1699(5) 0.0642(7) 0.080 Uiso 1 1 d
H9C H -0.1881(5) 0.1887(5) 0.0163(7) 0.080 Uiso 1 1 d
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.033(1) 0.033(1) 0.068(1) 0.006(1) -0.006(1) 0.001(1)
Te1 0.040(1) 0.030(1) 0.060(1) -0.001(1) 0.006(1) -0.002(1)
Cl1 0.041(1) 0.058(1) 0.160(2) 0.019(1) -0.009(1) -0.013(1)
N1 0.040(2) 0.042(2) 0.069(3) 0.007(2) -0.002(2) 0.009(2)
C1 0.034(3) 0.046(3) 0.055(4) -0.010(2) 0.001(2) -0.004(2)
C2 0.045(3) 0.034(2) 0.064(4) 0.001(2) 0.011(3) -0.001(2)
C3 0.057(3) 0.048(3) 0.063(4) -0.005(3) 0.011(3) 0.000(3)
C4 0.067(5) 0.072(5) 0.084(6) -0.030(4) 0.019(4) -0.010(4)
C5 0.060(4) 0.080(5) 0.059(4) -0.010(3) -0.005(3) -0.002(4)
C6 0.041(3) 0.054(3) 0.080(5) -0.014(3) -0.002(3) -0.004(2)
C7 0.061(4) 0.032(3) 0.083(5) 0.006(3) 0.015(3) 0.012(3)
C8 0.047(4) 0.062(4) 0.093(6) 0.002(4) 0.011(4) 0.007(3)
C9 0.070(5) 0.063(4) 0.092(6) 0.006(4) -0.023(4) 0.027(4)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 Pd1 Cl1 96.69(14)
N1 Pd1 Te1 92.17(13)
Cl1 Pd1 Te1 169.88(5)
N1 Pd1 Te1#1 172.75(13)
Cl1 Pd1 Te1#1 90.13(5)
Te1 Pd1 Te1#1 80.83(2)
C1 Te1 Pd1 84.4(2)
C1 Te1 Pd1#1 106.2(2)
Pd1 Te1 Pd1#1 97.47(2)
C8 N1 C7 110.5(6)
C8 N1 C9 108.7(6)
C7 N C9 106.9(5)
C8 N1 Pd1 110.7(4)
C7 N1 Pd1 112.9(3)
C9 N1 Pd1 106.9(4)
C2 C1 C6 120.5(6)
C2 C1 Te1 117.6(5)
C6 C1 Te1 121.9(4)
C3 C2 C1 119.6(6)
C3 C2 C7 121.1(6)
C1 C2 C7 119.3(6)
C4 C3 C2 119.7(6)
C3 C4 C5 121.8(7)
C6 C5 C4 119.1(7)
C5 C6 C1 119.1(6)
N1 C7 C2 114.2(5)
Cl3D Cl1D Cl1D#2 93.4(8)
Cl3D Cl1D C1D 61.6(8)
C1D#2 Cl1D C1D 36.9(9)
Cl2D#2 Cl2D C1D 93.5(9)
Cl2D#2 Cl2D C1D#2 46.0(5)
C1D Cl2D C1D#2 47.8(12)
Cl1D Cl3D C1D 93.3(9)
Cl1D Cl3D C1D#2 63.7(7)
C1D Cl3D C1D#2 35.5(9)
Cl2D C1D C1D#2 86.2(9)
Cl2D C1D Cl2D#2 40.5(7)
C1D#2 C1D Cl2D#2 46.0(5)
Cl2D C1D Cl3D 123.0(13)
C1D#2 C1D Cl3D 89(2)
Cl2D#2 C1D Cl3D 109.0(10)
Cl2D C1D Cl1D#2 128.6(13)
C1D#2 C1D Cl1D#2 75.3(11)
Cl2D#2 C1D Cl1D#2 109.3(9)
Cl3D C1D Cl1D#2 104.4(9)
Cl2D C1D Cl1D 130.5(12)
C1D#2 C1D Cl1D 67.8(11)
Cl2D#2 C1D Cl1D 100.3(8)
Cl3D C1D Cl1D 25.0(3)
Cl1D#2 C1D Cl1D 85.9(7)
Cl2D C1D Cl3D#2 110.4(12)
C1D#2 C1D Cl3D#2 55.5(12)
Cl2D#2 C1D Cl3D#2 86.0(7)
Cl3D C1D Cl3D#2 112.8(9)
Cl1D#2 C1D Cl3D#2 23.3(3)
Cl1D C1D Cl3D#2 89.2(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 N1 2.222(5)
Pd1 Cl1 2.360(2)
Pd1 Te1 2.5323(6)
Pd1 Te1#1 2.5464(6)
Te1 C1 2.132(6)
Te1 Pd1#1 2.5464(6)
N1 C8 1.467(9)
N1 C7 1.492(9)
N1 C9 1.496(9)
C1 C2 1.390(8)
C1 C6 1.400(9)
C2 C3 1.367(9)
C2 C7 1.506(10)
C3 C4 1.371(11)
C4 C5 1.381(10)
C5 C6 1.382(10)
Cl1D Cl3D 0.841(7)
Cl1D C1D#2 1.90(2)
Cl1D C1D 1.98(2)
Cl2D Cl2D#2 1.080(13)
Cl2D C1D 1.20(2)
Cl2D C1D#2 1.66(2)
Cl3D C1D 1.75(2)
Cl3D C1D#2 2.12(2)
C1D C1D#2 1.23(3)
C1D Cl2D#2 1.66(2)
C1D Cl1D#2 1.90(2)
C1D Cl3D#2 2.12(2)
