#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:38:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179149 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/10/4311011.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_4311011
loop_
_publ_author_name
'Thomas Devic'
'Patrick Batail'
'Marc Fourmigué'
'Narcis Avarvari'
_publ_section_title
;
 Unexpected Reactivity of PdCl2 and PtCl2 Complexes of the Unsaturated
 Diphosphineo-Me2TTF(PPh2)2 toward Chloride Abstraction with Thallium
 Triflate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3136
_journal_page_last               3141
_journal_paper_doi               10.1021/ic035447y
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         C34H28Cl8P2PdS4
_chemical_formula_sum            'C34 H28 Cl8 P2 Pd S4'
_chemical_formula_weight         1016.74
_chemical_name_common            'DM-TTF-(PPh2)2PdCl2, 2CHCl3'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                90.00
_cell_angle_beta                 118.152(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0352(13)
_cell_length_b                   15.7744(11)
_cell_length_c                   17.8266(14)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      1.85
_cell_volume                     4223.7(6)
_computing_cell_refinement       'CELL, Stoe-IPDS'
_computing_data_collection       'EXPOSE, Stoe-IPDS'
_computing_data_reduction        'INTEGRATE, Stoe-IPDS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       'rotation, phi incr. 1.3'
_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  0.1072
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34575
_diffrn_reflns_theta_full        25.86
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         4.146
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0892
_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)+(0.1213P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2695
_refine_ls_wR_factor_ref         0.2806
_reflns_number_gt                4605
_reflns_number_total             8099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035447ysi20040211_051635_1.cif
_cod_data_source_block           P2PdCl2
_cod_original_cell_volume        4223.7(5)
_cod_database_code               4311011
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.99130(5) 0.50421(4) 0.23887(5) 0.0311(3) Uani 1 1 d . . .
Cl1 Cl 1.0891(2) 0.60827(17) 0.3274(2) 0.0527(8) Uani 1 1 d . . .
Cl2 Cl 0.88830(19) 0.59870(17) 0.1392(2) 0.0502(7) Uani 1 1 d . . .
P1 P 0.90869(17) 0.39938(16) 0.15621(15) 0.0297(6) Uani 1 1 d . . .
P2 P 1.07969(17) 0.40769(15) 0.32992(16) 0.0292(6) Uani 1 1 d . . .
S1 S 0.9229(2) 0.20084(17) 0.16658(17) 0.0515(8) Uani 1 1 d . . .
S2 S 1.0803(2) 0.21055(17) 0.33788(17) 0.0488(8) Uani 1 1 d . . .
S3 S 0.9348(2) -0.00834(18) 0.1850(2) 0.0540(8) Uani 1 1 d . . .
S4 S 1.0879(2) 0.01003(18) 0.3531(2) 0.0557(8) Uani 1 1 d . . .
C1 C 0.9632(6) 0.3007(6) 0.2103(5) 0.0262(19) Uani 1 1 d . . .
C2 C 1.0362(6) 0.3045(6) 0.2889(5) 0.027(2) Uani 1 1 d . . .
C3 C 1.0022(7) 0.1458(6) 0.2544(7) 0.041(2) Uani 1 1 d . . .
C4 C 1.0051(8) 0.0620(6) 0.2624(7) 0.045(3) Uani 1 1 d . . .
C5 C 0.9826(7) -0.1016(6) 0.2361(6) 0.035(2) Uani 1 1 d . . .
C6 C 1.0537(8) -0.0944(6) 0.3152(6) 0.036(2) Uani 1 1 d . . .
C7 C 0.9456(12) -0.1844(8) 0.1950(11) 0.084(5) Uani 1 1 d . . .
H7A H 0.8962 -0.1749 0.1396 0.127 Uiso 1 1 calc R . .
H7B H 0.9258 -0.2156 0.2292 0.127 Uiso 1 1 calc R . .
H7C H 0.9908 -0.2161 0.1897 0.127 Uiso 1 1 calc R . .
C8 C 1.1138(13) -0.1623(9) 0.3749(12) 0.101(6) Uani 1 1 d . . .
H8A H 1.1577 -0.1364 0.4264 0.151 Uiso 1 1 calc R . .
H8B H 1.1429 -0.1923 0.3480 0.151 Uiso 1 1 calc R . .
H8C H 1.0788 -0.2013 0.3881 0.151 Uiso 1 1 calc R . .
C9 C 0.9049(7) 0.3946(6) 0.0544(6) 0.038(2) Uani 1 1 d . . .
C10 C 0.9799(8) 0.3659(9) 0.0484(8) 0.058(3) Uani 1 1 d . . .
H10 H 1.0298 0.3473 0.0970 0.070 Uiso 1 1 calc R . .
C11 C 0.9804(11) 0.3650(10) -0.0286(9) 0.069(4) Uani 1 1 d . . .
H11 H 1.0304 0.3456 -0.0316 0.082 Uiso 1 1 calc R . .
C12 C 0.9084(12) 0.3924(11) -0.1002(10) 0.084(5) Uani 1 1 d . . .
H12 H 0.9085 0.3914 -0.1523 0.101 Uiso 1 1 calc R . .
C13 C 0.8364(11) 0.4211(11) -0.0947(9) 0.083(5) Uani 1 1 d . . .
H13 H 0.7880 0.4404 -0.1442 0.099 Uiso 1 1 calc R . .
C14 C 0.8307(9) 0.4234(9) -0.0190(8) 0.064(4) Uani 1 1 d . . .
H14 H 0.7800 0.4432 -0.0175 0.077 Uiso 1 1 calc R . .
C15 C 0.7962(7) 0.3920(6) 0.1402(6) 0.036(2) Uani 1 1 d . . .
C16 C 0.7710(9) 0.4376(9) 0.1914(8) 0.062(4) Uani 1 1 d . . .
H16 H 0.8109 0.4750 0.2316 0.074 Uiso 1 1 calc R . .
C17 C 0.6856(10) 0.4277(12) 0.1831(11) 0.093(6) Uani 1 1 d . . .
H17 H 0.6685 0.4587 0.2174 0.112 Uiso 1 1 calc R . .
C18 C 0.6268(9) 0.3717(11) 0.1236(9) 0.072(4) Uani 1 1 d . . .
H18 H 0.5696 0.3658 0.1169 0.086 Uiso 1 1 calc R . .
C19 C 0.6522(8) 0.3252(10) 0.0747(9) 0.066(4) Uani 1 1 d . . .
H19 H 0.6126 0.2869 0.0354 0.080 Uiso 1 1 calc R . .
C20 C 0.7371(8) 0.3342(8) 0.0830(8) 0.057(3) Uani 1 1 d . . .
H20 H 0.7542 0.3013 0.0500 0.068 Uiso 1 1 calc R . .
C21 C 1.1925(7) 0.3985(6) 0.3441(6) 0.038(2) Uani 1 1 d . . .
C22 C 1.2584(9) 0.3539(8) 0.4126(9) 0.061(3) Uani 1 1 d . . .
H22 H 1.2476 0.3333 0.4557 0.074 Uiso 1 1 calc R . .
C23 C 1.3393(10) 0.3410(11) 0.4152(11) 0.081(5) Uani 1 1 d . . .
H23 H 1.3832 0.3097 0.4593 0.097 Uiso 1 1 calc R . .
C24 C 1.3544(10) 0.3731(15) 0.3549(12) 0.105(7) Uani 1 1 d . . .
H24 H 1.4103 0.3651 0.3588 0.126 Uiso 1 1 calc R . .
C25 C 1.2924(10) 0.4175(11) 0.2871(12) 0.088(5) Uani 1 1 d . . .
H25 H 1.3052 0.4387 0.2454 0.105 Uiso 1 1 calc R . .
C26 C 1.2104(9) 0.4297(9) 0.2825(10) 0.068(4) Uani 1 1 d . . .
H26 H 1.1667 0.4596 0.2369 0.082 Uiso 1 1 calc R . .
C27 C 1.0883(7) 0.4122(7) 0.4346(7) 0.039(2) Uani 1 1 d . . .
C28 C 1.0233(7) 0.3751(7) 0.4493(7) 0.046(3) Uani 1 1 d . . .
H28 H 0.9781 0.3442 0.4060 0.055 Uiso 1 1 calc R . .
C29 C 1.0239(9) 0.3830(9) 0.5260(8) 0.060(3) Uani 1 1 d . . .
H29 H 0.9769 0.3617 0.5331 0.072 Uiso 1 1 calc R . .
C30 C 1.0949(9) 0.4230(9) 0.5933(7) 0.060(3) Uani 1 1 d . . .
H30 H 1.0995 0.4227 0.6474 0.072 Uiso 1 1 calc R . .
C31 C 1.1570(10) 0.4622(10) 0.5791(9) 0.073(4) Uani 1 1 d . . .
H31 H 1.2020 0.4929 0.6228 0.088 Uiso 1 1 calc R . .
C32 C 1.1552(9) 0.4574(9) 0.5007(8) 0.060(3) Uani 1 1 d . . .
H32 H 1.1988 0.4845 0.4923 0.072 Uiso 1 1 calc R . .
Cl3 Cl 0.1847(7) 0.1920(8) 0.1959(5) 0.236(6) Uani 1 1 d . . .
Cl4 Cl 0.1796(5) 0.2257(8) 0.0438(5) 0.212(5) Uani 1 1 d . . .
Cl5 Cl 0.0920(8) 0.0868(7) 0.0578(10) 0.338(10) Uani 1 1 d . . .
C33 C 0.1800(12) 0.1454(12) 0.1096(12) 0.093(5) Uani 1 1 d . . .
H33 H 0.2333 0.1105 0.1265 0.112 Uiso 1 1 calc R . .
Cl6 Cl 0.4119(4) 0.3651(5) 0.9208(5) 0.152(3) Uani 1 1 d . . .
Cl7 Cl 0.3071(4) 0.2236(4) 0.9163(4) 0.129(2) Uani 1 1 d . . .
Cl8 Cl 0.2763(7) 0.3089(7) 0.7641(4) 0.200(4) Uani 1 1 d . . .
C34 C 0.3089(10) 0.3212(12) 0.8710(9) 0.087(5) Uani 1 1 d . . .
H34 H 0.2669 0.3595 0.8770 0.104 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
S S 0.1246 0.1234 '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
P2 Pd1 P1 88.47(9) . . ?
P2 Pd1 Cl1 88.07(10) . . ?
P1 Pd1 Cl1 175.11(11) . . ?
P2 Pd1 Cl2 175.43(10) . . ?
P1 Pd1 Cl2 87.55(10) . . ?
Cl1 Pd1 Cl2 96.03(11) . . ?
C9 P1 C15 108.0(5) . . ?
C9 P1 C1 105.3(4) . . ?
C15 P1 C1 105.4(4) . . ?
C9 P1 Pd1 114.4(4) . . ?
C15 P1 Pd1 116.5(3) . . ?
C1 P1 Pd1 106.1(3) . . ?
C2 P2 C27 105.9(5) . . ?
C2 P2 C21 100.9(5) . . ?
C27 P2 C21 107.1(5) . . ?
C2 P2 Pd1 108.5(3) . . ?
C27 P2 Pd1 115.2(4) . . ?
C21 P2 Pd1 117.7(3) . . ?
C3 S1 C1 94.2(4) . . ?
C2 S2 C3 95.5(4) . . ?
C5 S3 C4 98.6(5) . . ?
C4 S4 C6 96.1(5) . . ?
C2 C1 S1 118.2(7) . . ?
C2 C1 P1 119.4(7) . . ?
S1 C1 P1 122.4(5) . . ?
C1 C2 S2 117.1(7) . . ?
C1 C2 P2 117.3(7) . . ?
S2 C2 P2 125.6(5) . . ?
C4 C3 S1 124.5(9) . . ?
C4 C3 S2 120.4(9) . . ?
S1 C3 S2 115.1(6) . . ?
C3 C4 S3 125.0(9) . . ?
C3 C4 S4 122.3(9) . . ?
S3 C4 S4 112.6(6) . . ?
C6 C5 C7 123.2(10) . . ?
C6 C5 S3 116.3(7) . . ?
C7 C5 S3 120.4(9) . . ?
C5 C6 C8 130.0(11) . . ?
C5 C6 S4 116.4(7) . . ?
C8 C6 S4 113.4(10) . . ?
C14 C9 C10 119.1(10) . . ?
C14 C9 P1 121.3(9) . . ?
C10 C9 P1 119.5(8) . . ?
C11 C10 C9 120.9(12) . . ?
C12 C11 C10 120.3(14) . . ?
C13 C12 C11 119.2(13) . . ?
C12 C13 C14 123.8(14) . . ?
C9 C14 C13 116.7(12) . . ?
C16 C15 C20 118.9(10) . . ?
C16 C15 P1 120.1(8) . . ?
C20 C15 P1 120.6(8) . . ?
C15 C16 C17 120.3(12) . . ?
C18 C17 C16 119.6(13) . . ?
C19 C18 C17 120.3(13) . . ?
C18 C19 C20 120.5(12) . . ?
C15 C20 C19 120.4(12) . . ?
C26 C21 C22 119.5(11) . . ?
C26 C21 P2 118.8(9) . . ?
C22 C21 P2 121.5(9) . . ?
C23 C22 C21 119.0(13) . . ?
C24 C23 C22 119.6(15) . . ?
C23 C24 C25 123.5(15) . . ?
C24 C25 C26 117.8(14) . . ?
C21 C26 C25 120.6(14) . . ?
C28 C27 C32 117.8(10) . . ?
C28 C27 P2 119.8(8) . . ?
C32 C27 P2 122.2(9) . . ?
C29 C28 C27 121.5(11) . . ?
C28 C29 C30 119.8(12) . . ?
C31 C30 C29 119.1(11) . . ?
C30 C31 C32 121.1(13) . . ?
C31 C32 C27 120.3(13) . . ?
Cl5 C33 Cl3 113.8(14) . . ?
Cl5 C33 Cl4 108.9(12) . . ?
Cl3 C33 Cl4 106.6(12) . . ?
Cl6 C34 Cl8 109.8(11) . . ?
Cl6 C34 Cl7 110.9(8) . . ?
Cl8 C34 Cl7 110.2(11) . . ?
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 P2 2.217(3) . ?
Pd1 P1 2.220(3) . ?
Pd1 Cl1 2.341(3) . ?
Pd1 Cl2 2.349(3) . ?
P1 C9 1.786(10) . ?
P1 C15 1.802(10) . ?
P1 C1 1.836(9) . ?
P2 C2 1.795(9) . ?
P2 C27 1.803(11) . ?
P2 C21 1.822(11) . ?
S1 C3 1.741(11) . ?
S1 C1 1.748(9) . ?
S2 C2 1.704(9) . ?
S2 C3 1.778(11) . ?
S3 C5 1.720(10) . ?
S3 C4 1.735(11) . ?
S4 C4 1.766(12) . ?
S4 C6 1.771(10) . ?
C1 C2 1.367(12) . ?
C3 C4 1.330(15) . ?
C5 C6 1.363(14) . ?
C5 C7 1.483(15) . ?
C6 C8 1.518(15) . ?
C9 C14 1.399(15) . ?
C9 C10 1.407(15) . ?
C10 C11 1.376(17) . ?
C11 C12 1.36(2) . ?
C12 C13 1.35(2) . ?
C13 C14 1.400(18) . ?
C15 C16 1.381(15) . ?
C15 C20 1.384(15) . ?
C16 C17 1.399(18) . ?
C17 C18 1.38(2) . ?
C18 C19 1.36(2) . ?
C19 C20 1.390(17) . ?
C21 C26 1.364(16) . ?
C21 C22 1.396(16) . ?
C22 C23 1.371(19) . ?
C23 C24 1.32(2) . ?
C24 C25 1.36(2) . ?
C25 C26 1.373(18) . ?
C27 C28 1.382(15) . ?
C27 C32 1.388(16) . ?
C28 C29 1.369(16) . ?
C29 C30 1.389(18) . ?
C30 C31 1.349(19) . ?
C31 C32 1.385(18) . ?
Cl3 C33 1.67(2) . ?
Cl4 C33 1.72(2) . ?
Cl5 C33 1.63(2) . ?
Cl6 C34 1.696(19) . ?
Cl7 C34 1.75(2) . ?
Cl8 C34 1.725(15) . ?
