#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:10:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180028 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/22/7032204.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_7032204
loop_
_publ_author_name
'Kolay, Siddhartha'
'Kumar, Mukesh'
'Wadawale, Amey'
'Das, Dasarathi'
'Jain, Vimal K.'
_publ_section_title
;
 Cyclopalladation of telluro ether ligands: synthesis, reactivity and
 structural characterization.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16056
_journal_page_last               16065
_journal_paper_doi               10.1039/c4dt02200a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C40 H50 Cl2 N2 Pd Te2'
_chemical_formula_weight         991.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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-97
_cell_angle_alpha                90
_cell_angle_beta                 100.8045(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.85135(16)
_cell_length_b                   10.39083(17)
_cell_length_c                   23.3718(5)
_cell_measurement_reflns_used    10487
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      69.7880
_cell_measurement_theta_min      4.6680
_cell_volume                     2111.47(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  'WinGX 1.7.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12977
_diffrn_reflns_theta_full        69.91
_diffrn_reflns_theta_max         69.91
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    15.596
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0459
_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)+(0.0724P)²+3.3103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                3585
_reflns_number_total             3981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02200a2.cif
_cod_data_source_block           trans-[PdCl2(TeMes2)2]-1
_cod_depositor_comments
'Adding full bibliography for 7032199--7032205.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7032204
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.7868(6) 0.0596(5) 0.1281(2) 0.0472(11) Uani 1 1 d .
C1S C 0.3482(15) 0.5083(9) 0.0562(7) 0.113(4) Uani 1 1 d .
C2 C 0.6685(6) 0.1084(5) 0.0854(2) 0.0477(11) Uani 1 1 d .
C2S C 0.2133(18) 0.5333(10) 0.0146(6) 0.140(5) Uani 1 1 d .
H2S1 H 0.1464 0.4599 0.0117 0.210 Uiso 1 1 calc R
H2S2 H 0.2404 0.5497 -0.0226 0.210 Uiso 1 1 calc R
H2S3 H 0.1617 0.6070 0.0265 0.210 Uiso 1 1 calc R
C3 C 0.5397(7) 0.1586(6) 0.1038(2) 0.0575(13) Uani 1 1 d .
H3 H 0.4602 0.1913 0.0759 0.069 Uiso 1 1 calc R
C4 C 0.5242(7) 0.1622(6) 0.1612(3) 0.0622(15) Uani 1 1 d .
C5 C 0.6446(7) 0.1145(7) 0.2023(3) 0.0668(16) Uani 1 1 d .
H5 H 0.6371 0.1179 0.2414 0.080 Uiso 1 1 calc R
C6 C 0.7751(7) 0.0622(6) 0.1875(2) 0.0558(13) Uani 1 1 d .
C8 C 0.6713(7) 0.1095(7) 0.0218(2) 0.0627(15) Uani 1 1 d .
H8A H 0.7538 0.1634 0.0147 0.094 Uiso 1 1 calc R
H8B H 0.5753 0.1423 0.0009 0.094 Uiso 1 1 calc R
H8C H 0.6864 0.0234 0.0090 0.094 Uiso 1 1 calc R
C9 C 0.3818(8) 0.2185(9) 0.1787(3) 0.088(2) Uani 1 1 d .
H9A H 0.3752 0.1898 0.2172 0.132 Uiso 1 1 calc R
H9B H 0.2922 0.1908 0.1518 0.132 Uiso 1 1 calc R
H9C H 0.3877 0.3108 0.1783 0.132 Uiso 1 1 calc R
C10 C 0.9767(6) -0.2169(5) 0.1287(2) 0.0475(11) Uani 1 1 d .
C11 C 0.8383(6) -0.2851(5) 0.1194(2) 0.0514(12) Uani 1 1 d .
C12 C 0.8426(7) -0.4157(6) 0.1341(2) 0.0575(13) Uani 1 1 d .
H12 H 0.7510 -0.4617 0.1285 0.069 Uiso 1 1 calc R
C13 C 0.9783(9) -0.4788(6) 0.1566(3) 0.0645(16) Uani 1 1 d .
C14 C 1.1122(8) -0.4093(7) 0.1638(3) 0.0650(16) Uani 1 1 d .
H14 H 1.2043 -0.4513 0.1781 0.078 Uiso 1 1 calc R
C15 C 1.1163(6) -0.2786(6) 0.1507(2) 0.0554(13) Uani 1 1 d .
C16 C 1.2689(7) -0.2108(8) 0.1597(4) 0.088(2) Uani 1 1 d .
H16A H 1.2812 -0.1697 0.1240 0.132 Uiso 1 1 calc R
H16B H 1.3501 -0.2722 0.1710 0.132 Uiso 1 1 calc R
H16C H 1.2729 -0.1472 0.1897 0.132 Uiso 1 1 calc R
C17 C 0.6859(6) -0.2287(6) 0.0917(3) 0.0742(19) Uani 1 1 d .
H17A H 0.6445 -0.1805 0.1203 0.111 Uiso 1 1 calc R
H17B H 0.6162 -0.2967 0.0768 0.111 Uiso 1 1 calc R
H17C H 0.6996 -0.1728 0.0604 0.111 Uiso 1 1 calc R
C18 C 0.9757(11) -0.6209(7) 0.1712(4) 0.097(3) Uani 1 1 d .
H18A H 1.0544 -0.6648 0.1556 0.145 Uiso 1 1 calc R
H18B H 0.8771 -0.6564 0.1545 0.145 Uiso 1 1 calc R
H18C H 0.9939 -0.6316 0.2127 0.145 Uiso 1 1 calc R
N1S N 0.4496(18) 0.4904(11) 0.0918(9) 0.200(8) Uani 1 1 d .
C7 C 0.8991(11) 0.0102(8) 0.2350(3) 0.088(3) Uani 1 1 d .
H7A H 0.8856 0.0442 0.2719 0.133 Uiso 1 1 calc R
H7B H 0.9981 0.0353 0.2276 0.133 Uiso 1 1 calc R
H7C H 0.8927 -0.0820 0.2358 0.133 Uiso 1 1 calc R
Cl1 Cl 1.0858(2) 0.20577(14) 0.02346(7) 0.0685(4) Uani 1 1 d .
Pd1 Pd 1.0000 0.0000 0.0000 0.04440(17) Uani 1 2 d S
Te1 Te 0.99599(4) -0.01692(3) 0.109911(14) 0.04658(15) 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 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.1759 6.3531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
C2 C1 C6 120.8(5) . .
C2 C1 Te1 123.7(4) . .
C6 C1 Te1 115.5(4) . .
N1S C1S C2S 176(2) . .
C3 C2 C1 117.5(5) . .
C3 C2 C8 118.2(5) . .
C1 C2 C8 124.3(5) . .
C1S C2S H2S1 109.5 . .
C1S C2S H2S2 109.5 . .
H2S1 C2S H2S2 109.5 . .
C1S C2S H2S3 109.5 . .
H2S1 C2S H2S3 109.5 . .
H2S2 C2S H2S3 109.5 . .
C4 C3 C2 123.3(5) . .
C4 C3 H3 118.4 . .
C2 C3 H3 118.4 . .
C3 C4 C5 117.5(5) . .
C3 C4 C9 121.0(6) . .
C5 C4 C9 121.5(6) . .
C6 C5 C4 122.6(6) . .
C6 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
C5 C6 C1 118.3(5) . .
C5 C6 C7 119.0(6) . .
C1 C6 C7 122.7(6) . .
C2 C8 H8A 109.5 . .
C2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C4 C9 H9A 109.5 . .
C4 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C4 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 C15 120.8(5) . .
C11 C10 Te1 124.3(4) . .
C15 C10 Te1 114.9(4) . .
C10 C11 C12 118.1(5) . .
C10 C11 C17 124.0(5) . .
C12 C11 C17 117.8(5) . .
C13 C12 C11 122.4(6) . .
C13 C12 H12 118.8 . .
C11 C12 H12 118.8 . .
C14 C13 C12 117.8(6) . .
C14 C13 C18 122.3(7) . .
C12 C13 C18 119.9(7) . .
C13 C14 C15 123.0(6) . .
C13 C14 H14 118.5 . .
C15 C14 H14 118.5 . .
C14 C15 C10 117.9(6) . .
C14 C15 C16 119.1(5) . .
C10 C15 C16 123.0(6) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C11 C17 H17A 109.5 . .
C11 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C11 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C13 C18 H18A 109.5 . .
C13 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C13 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Cl1 Pd1 Cl1 180.00(11) . 3_755
Cl1 Pd1 Te1 96.22(4) . 3_755
Cl1 Pd1 Te1 83.78(4) 3_755 3_755
Cl1 Pd1 Te1 83.78(4) . .
Cl1 Pd1 Te1 96.22(4) 3_755 .
Te1 Pd1 Te1 180.000(15) 3_755 .
C1 Te1 C10 102.5(2) . .
C1 Te1 Pd1 110.36(13) . .
C10 Te1 Pd1 106.71(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.399(7) .
C1 C6 1.411(7) .
C1 Te1 2.130(5) .
C1S N1S 1.119(18) .
C1S C2S 1.415(17) .
C2 C3 1.393(8) .
C2 C8 1.491(7) .
C2S H2S1 0.9600 .
C2S H2S2 0.9600 .
C2S H2S3 0.9600 .
C3 C4 1.374(8) .
C3 H3 0.9300 .
C4 C5 1.386(9) .
C4 C9 1.514(9) .
C5 C6 1.377(9) .
C5 H5 0.9300 .
C6 C7 1.508(9) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 C11 1.396(7) .
C10 C15 1.402(7) .
C10 Te1 2.137(5) .
C11 C12 1.398(8) .
C11 C17 1.502(8) .
C12 C13 1.383(9) .
C12 H12 0.9300 .
C13 C14 1.370(10) .
C13 C18 1.517(9) .
C14 C15 1.394(9) .
C14 H14 0.9300 .
C15 C16 1.503(9) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
Cl1 Pd1 2.3006(14) .
Pd1 Cl1 2.3006(14) 3_755
Pd1 Te1 2.5817(3) 3_755
Pd1 Te1 2.5817(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C6 C1 C2 C3 -0.3(8) .
Te1 C1 C2 C3 -178.3(4) .
C6 C1 C2 C8 -179.9(6) .
Te1 C1 C2 C8 2.0(8) .
C1 C2 C3 C4 0.0(9) .
C8 C2 C3 C4 179.7(6) .
C2 C3 C4 C5 0.8(9) .
C2 C3 C4 C9 179.7(6) .
C3 C4 C5 C6 -1.4(10) .
C9 C4 C5 C6 179.7(7) .
C4 C5 C6 C1 1.2(10) .
C4 C5 C6 C7 -178.8(7) .
C2 C1 C6 C5 -0.3(9) .
Te1 C1 C6 C5 177.9(5) .
C2 C1 C6 C7 179.7(6) .
Te1 C1 C6 C7 -2.1(8) .
C15 C10 C11 C12 1.6(8) .
Te1 C10 C11 C12 -179.7(4) .
C15 C10 C11 C17 -175.0(6) .
Te1 C10 C11 C17 3.7(8) .
C10 C11 C12 C13 -0.8(8) .
C17 C11 C12 C13 176.1(6) .
C11 C12 C13 C14 -0.7(9) .
C11 C12 C13 C18 -179.6(6) .
C12 C13 C14 C15 1.4(10) .
C18 C13 C14 C15 -179.8(7) .
C13 C14 C15 C10 -0.6(9) .
C13 C14 C15 C16 -179.5(7) .
C11 C10 C15 C14 -1.0(8) .
Te1 C10 C15 C14 -179.8(4) .
C11 C10 C15 C16 177.9(6) .
Te1 C10 C15 C16 -1.0(8) .
C2 C1 Te1 C10 -111.8(5) .
C6 C1 Te1 C10 70.1(5) .
C2 C1 Te1 Pd1 1.6(5) .
C6 C1 Te1 Pd1 -176.6(4) .
C11 C10 Te1 C1 33.8(5) .
C15 C10 Te1 C1 -147.4(4) .
C11 C10 Te1 Pd1 -82.2(4) .
C15 C10 Te1 Pd1 96.6(4) .
Cl1 Pd1 Te1 C1 84.06(16) .
Cl1 Pd1 Te1 C1 -95.94(16) 3_755
Te1 Pd1 Te1 C1 -122(100) 3_755
Cl1 Pd1 Te1 C10 -165.35(15) .
Cl1 Pd1 Te1 C10 14.65(15) 3_755
Te1 Pd1 Te1 C10 -12(100) 3_755
