#------------------------------------------------------------------------------
#$Date: 2019-11-23 01:42:41 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231789 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/64/4346466.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_4346466
loop_
_publ_author_name
'Wrixon, Justin D.'
'Hayward, John J.'
'Rawson, Jeremy M.'
_publ_section_title
;
 Phosphine control of the oxidative addition chemistry of tetrathiocins to
 palladium(0): characterization of mono-, di-, and hexanuclear
 palladium(II) dithiolate complexes.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9384
_journal_page_last               9386
_journal_paper_doi               10.1021/acs.inorgchem.5b01555
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C52 H46 O4 P2 Pd2 S4, 3(C H2 Cl2)'
_chemical_formula_sum            'C55 H52 Cl6 O4 P2 Pd2 S4'
_chemical_formula_weight         1392.714
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.9591(17)
_cell_length_b                   20.351(2)
_cell_length_c                   8.4374(8)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.33
_cell_volume                     2912.0(5)
_computing_cell_refinement       'Bruker APEX-II'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker APEX-II'
_computing_molecular_graphics    'Mercury v3.0'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            33406
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.8132
_exptl_absorpt_correction_T_min  0.7198
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0238P)²+1.5805P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                6538
_reflns_number_total             6634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01555_si_003.cif
_cod_data_source_block           jw004
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2912.1(5)
_cod_original_sg_symbol_H-M      P2(1)2(1)2
_cod_database_code               4346466
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -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
Pd Pd 0.482120(8) 0.429957(6) 0.576194(16) 0.01426(4) Uani 1 1 d . . .
P1 P 0.37987(3) 0.38091(2) 0.44807(6) 0.01657(10) Uani 1 1 d . . .
S1 S 0.58613(3) 0.48306(2) 0.70188(6) 0.01594(9) Uani 1 1 d . . .
O1 O 0.88613(8) 0.47629(7) 0.5867(2) 0.0257(3) Uani 1 1 d . . .
C1 C 0.67000(11) 0.45252(9) 0.6017(2) 0.0166(4) Uani 1 1 d . . .
O2 O 0.87018(8) 0.38659(8) 0.37244(19) 0.0254(3) Uani 1 1 d . . .
S2 S 0.57057(3) 0.36526(2) 0.44658(7) 0.02012(10) Uani 1 1 d . . .
C2 C 0.74492(11) 0.47765(10) 0.6391(2) 0.0176(4) Uani 1 1 d . . .
H2 H 0.7501 0.5110 0.7171 0.021 Uiso 1 1 calc R . .
C3 C 0.81064(11) 0.45394(9) 0.5630(3) 0.0184(4) Uani 1 1 d . . .
C4 C 0.80234(11) 0.40451(9) 0.4472(3) 0.0193(4) Uani 1 1 d . . .
C5 C 0.72909(11) 0.37895(9) 0.4148(3) 0.0198(4) Uani 1 1 d . . .
H5 H 0.7242 0.3449 0.3385 0.024 Uiso 1 1 calc R . .
C6 C 0.66180(11) 0.40217(9) 0.4919(2) 0.0175(4) Uani 1 1 d . . .
C7 C 0.89443(14) 0.53257(12) 0.6854(4) 0.0374(6) Uani 1 1 d . . .
H7A H 0.8602 0.5678 0.6462 0.056 Uiso 1 1 calc R . .
H7B H 0.9494 0.5474 0.6839 0.056 Uiso 1 1 calc R . .
H7C H 0.8793 0.5213 0.7942 0.056 Uiso 1 1 calc R . .
C8 C 0.86281(14) 0.34101(12) 0.2447(3) 0.0313(5) Uani 1 1 d . . .
H8A H 0.8388 0.3003 0.2836 0.047 Uiso 1 1 calc R . .
H8B H 0.9151 0.3315 0.2011 0.047 Uiso 1 1 calc R . .
H8C H 0.8294 0.3600 0.1618 0.047 Uiso 1 1 calc R . .
C11 C 0.30266(10) 0.34900(9) 0.5764(3) 0.0185(4) Uani 1 1 d . . .
C12 C 0.24116(13) 0.31211(10) 0.5127(3) 0.0251(4) Uani 1 1 d . . .
H12 H 0.2403 0.3025 0.4026 0.030 Uiso 1 1 calc R . .
C13 C 0.18113(13) 0.28943(11) 0.6100(3) 0.0289(5) Uani 1 1 d . . .
H13 H 0.1385 0.2652 0.5660 0.035 Uiso 1 1 calc R . .
C14 C 0.18320(14) 0.30202(11) 0.7717(3) 0.0313(5) Uani 1 1 d . . .
H14 H 0.1417 0.2869 0.8379 0.038 Uiso 1 1 calc R . .
C15 C 0.24543(14) 0.33648(12) 0.8361(3) 0.0296(5) Uani 1 1 d . . .
H15 H 0.2475 0.3439 0.9471 0.036 Uiso 1 1 calc R . .
C16 C 0.30506(12) 0.36036(10) 0.7389(3) 0.0222(4) Uani 1 1 d . . .
H16 H 0.3476 0.3845 0.7835 0.027 Uiso 1 1 calc R . .
C21 C 0.40584(12) 0.30959(10) 0.3282(3) 0.0224(4) Uani 1 1 d . . .
C22 C 0.40903(14) 0.31280(13) 0.1639(3) 0.0318(5) Uani 1 1 d . . .
H22 H 0.3957 0.3523 0.1104 0.038 Uiso 1 1 calc R . .
C23 C 0.43186(16) 0.25763(14) 0.0784(4) 0.0433(6) Uani 1 1 d . . .
H23 H 0.4342 0.2597 -0.0340 0.052 Uiso 1 1 calc R . .
C24 C 0.45097(16) 0.20044(14) 0.1537(4) 0.0446(7) Uani 1 1 d . . .
H24 H 0.4664 0.1631 0.0936 0.054 Uiso 1 1 calc R . .
C25 C 0.44792(16) 0.19669(13) 0.3173(4) 0.0417(6) Uani 1 1 d . . .
H25 H 0.4605 0.1567 0.3696 0.050 Uiso 1 1 calc R . .
C26 C 0.42638(14) 0.25157(11) 0.4044(3) 0.0330(5) Uani 1 1 d . . .
H26 H 0.4257 0.2495 0.5168 0.040 Uiso 1 1 calc R . .
C31 C 0.33621(12) 0.43706(10) 0.3059(2) 0.0216(4) Uani 1 1 d . . .
C32 C 0.25679(13) 0.43907(12) 0.2657(3) 0.0308(5) Uani 1 1 d . . .
H32 H 0.2198 0.4119 0.3190 0.037 Uiso 1 1 calc R . .
C33 C 0.23219(18) 0.48162(15) 0.1460(3) 0.0447(7) Uani 1 1 d . . .
H33 H 0.1780 0.4830 0.1178 0.054 Uiso 1 1 calc R . .
C34 C 0.2841(2) 0.52128(13) 0.0687(3) 0.0447(7) Uani 1 1 d . . .
H34 H 0.2661 0.5496 -0.0132 0.054 Uiso 1 1 calc R . .
C35 C 0.3621(2) 0.52025(14) 0.1090(3) 0.0440(7) Uani 1 1 d . . .
H35 H 0.3985 0.5481 0.0558 0.053 Uiso 1 1 calc R . .
C36 C 0.38804(16) 0.47848(12) 0.2275(3) 0.0346(5) Uani 1 1 d . . .
H36 H 0.4423 0.4782 0.2555 0.041 Uiso 1 1 calc R . .
C1S C 0.12814(19) 0.19632(16) 0.1495(4) 0.0526(6) Uani 1 1 d D . .
H1S1 H 0.1064 0.1817 0.0465 0.063 Uiso 1 1 calc R . .
H1S2 H 0.1088 0.1660 0.2326 0.063 Uiso 1 1 calc R . .
Cl1 Cl 0.09515(5) 0.27627(5) 0.19044(10) 0.0605(2) Uani 1 1 d D . .
Cl2 Cl 0.23162(5) 0.19328(4) 0.14267(10) 0.05556(19) Uani 1 1 d D . .
C2S C 0.0000 0.5000 0.2818(5) 0.0526(6) Uani 0.50 1 d PD A -1
H2S1 H -0.0548 0.4953 0.3206 0.063 Uiso 0.50 1 calc PR A -1
H2S2 H 0.0278 0.5319 0.3506 0.063 Uiso 0.50 1 calc PR A -1
Cl3 Cl 0.00015(14) 0.52670(14) 0.0903(2) 0.0946(11) Uani 0.50 1 d PD A -1
Cl4 Cl 0.05180(9) 0.41823(9) 0.2859(4) 0.0930(9) Uani 0.50 1 d PD A -1
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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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
P1 Pd S2 91.159(19) . .
P1 Pd S1 178.137(19) . .
S2 Pd S1 89.314(19) . .
P1 Pd S1 99.695(19) . 2_665
S2 Pd S1 166.087(18) . 2_665
S1 Pd S1 79.57(2) . 2_665
P1 Pd Pd 126.013(14) . 2_665
S2 Pd Pd 115.386(15) . 2_665
S1 Pd Pd 52.220(12) . 2_665
S1 Pd Pd 50.951(13) 2_665 2_665
C31 P1 C11 108.95(9) . .
C31 P1 C21 103.48(10) . .
C11 P1 C21 102.71(9) . .
C31 P1 Pd 110.43(7) . .
C11 P1 Pd 115.00(7) . .
C21 P1 Pd 115.40(7) . .
C1 S1 Pd 103.24(7) . .
C1 S1 Pd 116.26(7) . 2_665
Pd S1 Pd 76.832(16) . 2_665
C3 O1 C7 116.36(16) . .
C6 C1 C2 120.59(17) . .
C6 C1 S1 119.88(14) . .
C2 C1 S1 119.48(15) . .
C4 O2 C8 116.73(16) . .
C6 S2 Pd 103.18(7) . .
C3 C2 C1 120.03(18) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
O1 C3 C2 124.87(18) . .
O1 C3 C4 115.51(17) . .
C2 C3 C4 119.58(17) . .
O2 C4 C5 124.75(18) . .
O2 C4 C3 115.33(17) . .
C5 C4 C3 119.91(18) . .
C4 C5 C6 121.21(19) . .
C4 C5 H5 119.4 . .
C6 C5 H5 119.4 . .
C1 C6 C5 118.61(17) . .
C1 C6 S2 123.18(15) . .
C5 C6 S2 118.21(15) . .
O1 C7 H7A 109.5 . .
O1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
O1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
O2 C8 H8A 109.5 . .
O2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
O2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C16 C11 C12 119.46(19) . .
C16 C11 P1 120.42(15) . .
C12 C11 P1 120.12(17) . .
C13 C12 C11 120.1(2) . .
C13 C12 H12 120.0 . .
C11 C12 H12 120.0 . .
C12 C13 C14 120.1(2) . .
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 . .
C15 C14 C13 120.0(2) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C14 C15 C16 120.2(2) . .
C14 C15 H15 119.9 . .
C16 C15 H15 119.9 . .
C15 C16 C11 120.1(2) . .
C15 C16 H16 119.9 . .
C11 C16 H16 119.9 . .
C26 C21 C22 119.5(2) . .
C26 C21 P1 118.75(18) . .
C22 C21 P1 121.72(18) . .
C23 C22 C21 119.4(3) . .
C23 C22 H22 120.3 . .
C21 C22 H22 120.3 . .
C24 C23 C22 120.9(3) . .
C24 C23 H23 119.5 . .
C22 C23 H23 119.5 . .
C23 C24 C25 120.2(3) . .
C23 C24 H24 119.9 . .
C25 C24 H24 119.9 . .
C24 C25 C26 119.6(3) . .
C24 C25 H25 120.2 . .
C26 C25 H25 120.2 . .
C25 C26 C21 120.4(3) . .
C25 C26 H26 119.8 . .
C21 C26 H26 119.8 . .
C36 C31 C32 118.7(2) . .
C36 C31 P1 116.09(17) . .
C32 C31 P1 125.11(17) . .
C31 C32 C33 119.0(2) . .
C31 C32 H32 120.5 . .
C33 C32 H32 120.5 . .
C34 C33 C32 121.5(3) . .
C34 C33 H33 119.3 . .
C32 C33 H33 119.3 . .
C33 C34 C35 119.9(2) . .
C33 C34 H34 120.1 . .
C35 C34 H34 120.1 . .
C34 C35 C36 119.8(3) . .
C34 C35 H35 120.1 . .
C36 C35 H35 120.1 . .
C35 C36 C31 121.1(2) . .
C35 C36 H36 119.4 . .
C31 C36 H36 119.4 . .
Cl1 C1S Cl2 110.95(17) . .
Cl1 C1S H1S1 109.4 . .
Cl2 C1S H1S1 109.4 . .
Cl1 C1S H1S2 109.4 . .
Cl2 C1S H1S2 109.4 . .
H1S1 C1S H1S2 108.0 . .
Cl3 C2S Cl4 107.4(2) . .
Cl3 C2S H2S1 110.2 . .
Cl4 C2S H2S1 110.2 . .
Cl3 C2S H2S2 110.2 . .
Cl4 C2S H2S2 110.2 . .
H2S1 C2S H2S2 108.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd P1 2.2742(5) .
Pd S2 2.2759(5) .
Pd S1 2.3247(5) .
Pd S1 2.3660(5) 2_665
Pd Pd 2.9148(4) 2_665
P1 C31 1.815(2) .
P1 C11 1.819(2) .
P1 C21 1.823(2) .
S1 C1 1.7673(19) .
S1 Pd 2.3660(5) 2_665
O1 C3 1.373(2) .
O1 C7 1.423(3) .
C1 C6 1.389(3) .
C1 C2 1.406(3) .
O2 C4 1.362(2) .
O2 C8 1.427(3) .
S2 C6 1.762(2) .
C2 C3 1.374(3) .
C2 H2 0.9500 .
C3 C4 1.409(3) .
C4 C5 1.374(3) .
C5 C6 1.396(3) .
C5 H5 0.9500 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C11 C16 1.391(3) .
C11 C12 1.393(3) .
C12 C13 1.387(3) .
C12 H12 0.9500 .
C13 C14 1.388(4) .
C13 H13 0.9500 .
C14 C15 1.379(4) .
C14 H14 0.9500 .
C15 C16 1.390(3) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C21 C26 1.389(3) .
C21 C22 1.389(3) .
C22 C23 1.389(3) .
C22 H22 0.9500 .
C23 C24 1.365(4) .
C23 H23 0.9500 .
C24 C25 1.383(4) .
C24 H24 0.9500 .
C25 C26 1.386(4) .
C25 H25 0.9500 .
C26 H26 0.9500 .
C31 C36 1.386(3) .
C31 C32 1.390(3) .
C32 C33 1.394(3) .
C32 H32 0.9500 .
C33 C34 1.361(4) .
C33 H33 0.9500 .
C34 C35 1.367(4) .
C34 H34 0.9500 .
C35 C36 1.384(3) .
C35 H35 0.9500 .
C36 H36 0.9500 .
C1S Cl1 1.755(4) .
C1S Cl2 1.757(3) .
C1S H1S1 0.9900 .
C1S H1S2 0.9900 .
C2S Cl3 1.704(4) .
C2S Cl4 1.8821(18) .
C2S H2S1 0.9900 .
C2S H2S2 0.9900 .
