#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:57:49 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178762 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/16/4101645.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_4101645
loop_
_publ_author_name
'Shen, Zhongliang'
'Jordan, Richard F.'
_publ_section_title
;
 Self-assembled tetranuclear palladium catalysts that produce high
 molecular weight linear polyethylene.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              52
_journal_page_last               53
_journal_paper_doi               10.1021/ja909473y
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C42 H38 Cl4 O12 P2 Pd2 S4'
_chemical_formula_weight         1279.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 110.23(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.764(5)
_cell_length_b                   14.101(7)
_cell_length_c                   18.639(7)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      1.86
_cell_volume                     2408(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0936
_diffrn_reflns_av_sigmaI/netI    0.0762
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21048
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.9510
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption corrections were made based on correspondance of
equivalent intensities usingprogram SADABS (G. Sheldrick, Bruker 
Analytical X-ray Systems, Madison, WI)
;
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.991
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.704
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0416P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                3252
_reflns_number_total             4266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909473y_si_006.cif
_cod_data_source_block           zhon03z
_cod_original_cell_volume        2408.0(19)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4101645
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 -0.06089(4) 0.35890(3) 0.95707(2) 0.01924(13) Uani 1 1 d . . .
S1 S 0.07524(14) 0.54310(9) 0.89943(8) 0.0209(3) Uani 1 1 d . . .
S2 S 0.29530(15) 0.68374(10) 1.19158(8) 0.0235(3) Uani 1 1 d . . .
P1 P 0.19838(14) 0.73774(9) 1.00813(8) 0.0178(3) Uani 1 1 d . . .
O1 O 0.0942(4) 0.4510(2) 0.9375(2) 0.0264(9) Uani 1 1 d . . .
O2 O 0.0139(4) 0.5404(3) 0.8190(2) 0.0274(9) Uani 1 1 d . . .
O3 O -0.0098(4) 0.6089(2) 0.9305(2) 0.0219(8) Uani 1 1 d . . .
O4 O 0.1317(4) 0.6815(2) 1.1519(2) 0.0224(8) Uani 1 1 d . . .
O5 O 0.3657(4) 0.6087(2) 1.1656(2) 0.0265(9) Uani 1 1 d . . .
O6 O 0.3280(4) 0.6919(3) 1.2715(2) 0.0302(9) Uani 1 1 d . . .
C1 C 0.3146(5) 0.8127(4) 1.0836(3) 0.0181(11) Uani 1 1 d . . .
C2 C 0.3489(5) 0.7908(4) 1.1603(3) 0.0203(12) Uani 1 1 d . . .
C3 C 0.4308(6) 0.8533(4) 1.2148(3) 0.0256(12) Uani 1 1 d . . .
H3 H 0.4546 0.8386 1.2674 0.026(11) Uiso 1 1 d R . .
C4 C 0.4793(6) 0.9380(4) 1.1936(3) 0.0277(13) Uani 1 1 d . . .
H4 H 0.5363 0.9806 1.2318 0.025(15) Uiso 1 1 d R . .
C5 C 0.4449(6) 0.9605(4) 1.1172(3) 0.0227(12) Uani 1 1 d . . .
C6 C 0.3609(5) 0.8975(4) 1.0631(3) 0.0219(12) Uani 1 1 d . . .
H6 H 0.3343 0.9131 1.0105 0.025(12) Uiso 1 1 d R . .
C7 C 0.4950(7) 1.0519(4) 1.0943(3) 0.0337(15) Uani 1 1 d . . .
H7A H 0.4452 1.0621 1.0394 0.042(18) Uiso 1 1 d R . .
H7B H 0.4721 1.1041 1.1229 0.032(16) Uiso 1 1 d R . .
H7C H 0.6007 1.0493 1.1055 0.032(14) Uiso 1 1 d R . .
C8 C 0.3078(5) 0.6688(3) 0.9667(3) 0.0183(11) Uani 1 1 d . . .
C9 C 0.2565(5) 0.5872(3) 0.9245(3) 0.0177(11) Uani 1 1 d . . .
C10 C 0.3444(6) 0.5356(4) 0.8948(3) 0.0225(12) Uani 1 1 d . . .
H10 H 0.3092 0.4786 0.8675 0.020(14) Uiso 1 1 d R . .
C11 C 0.4837(6) 0.5671(4) 0.9049(3) 0.0237(12) Uani 1 1 d . . .
H11 H 0.5451 0.5306 0.8856 0.000(11) Uiso 1 1 d R . .
C12 C 0.5347(5) 0.6505(4) 0.9426(3) 0.0242(12) Uani 1 1 d . . .
C13 C 0.4499(5) 0.6993(4) 0.9756(3) 0.0197(12) Uani 1 1 d . . .
H13 H 0.4878 0.7546 1.0048 0.015(13) Uiso 1 1 d R . .
C14 C 0.6807(6) 0.6893(4) 0.9466(4) 0.0328(15) Uani 1 1 d . . .
H14A H 0.7401 0.7019 1.0000 0.07(2) Uiso 1 1 d R . .
H14B H 0.7305 0.6429 0.9251 0.045(18) Uiso 1 1 d R . .
H14C H 0.6667 0.7484 0.9172 0.07(2) Uiso 1 1 d R . .
C15 C 0.0907(6) 0.8168(4) 0.9359(3) 0.0203(12) Uani 1 1 d . . .
C16 C -0.0136(5) 0.8715(4) 0.9519(3) 0.0257(13) Uani 1 1 d . . .
H16 H -0.0283 0.8651 0.9995 0.030(11) Uiso 1 1 d R . .
C17 C -0.0950(6) 0.9346(4) 0.8983(3) 0.0304(14) Uani 1 1 d . . .
H17 H -0.1668 0.9719 0.9089 0.036(17) Uiso 1 1 d R . .
C18 C -0.0743(6) 0.9447(4) 0.8297(3) 0.0303(14) Uani 1 1 d . . .
H18 H -0.1319 0.9883 0.7927 0.030(13) Uiso 1 1 d R . .
C19 C 0.0301(6) 0.8913(4) 0.8147(3) 0.0274(13) Uani 1 1 d . . .
H19 H 0.0463 0.8993 0.7677 0.027(15) Uiso 1 1 d R . .
C20 C 0.1106(6) 0.8273(4) 0.8664(3) 0.0241(13) Uani 1 1 d . . .
H20 H 0.1808 0.7895 0.8549 0.024(14) Uiso 1 1 d R . .
Cl1 Cl 0.70332(17) 0.77963(11) 0.67732(10) 0.0448(4) Uani 1 1 d . . .
Cl2 Cl 0.8077(2) 0.62534(12) 0.60773(11) 0.0524(5) Uani 1 1 d . . .
C21 C 0.8502(7) 0.7025(5) 0.6861(4) 0.0450(17) Uani 1 1 d . . .
H21A H 0.9380 0.7399 0.6896 0.09(3) Uiso 1 1 d R . .
H21B H 0.8725 0.6650 0.7338 0.038(17) Uiso 1 1 d 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'
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'
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
O4 Pd1 O3 176.32(14) 3_567 3_567 ?
O4 Pd1 O1 90.92(14) 3_567 . ?
O3 Pd1 O1 91.88(14) 3_567 . ?
O4 Pd1 P1 95.35(11) 3_567 3_567 ?
O3 Pd1 P1 81.69(11) 3_567 3_567 ?
O1 Pd1 P1 172.51(11) . 3_567 ?
O2 S1 O1 115.3(2) . . ?
O2 S1 O3 110.0(2) . . ?
O1 S1 O3 111.1(2) . . ?
O2 S1 C9 107.9(2) . . ?
O1 S1 C9 103.6(2) . . ?
O3 S1 C9 108.6(2) . . ?
O6 S2 O5 117.1(2) . . ?
O6 S2 O4 109.4(2) . . ?
O5 S2 O4 111.6(2) . . ?
O6 S2 C2 107.0(2) . . ?
O5 S2 C2 106.8(2) . . ?
O4 S2 C2 103.9(2) . . ?
C15 P1 C8 107.2(2) . . ?
C15 P1 C1 105.6(2) . . ?
C8 P1 C1 110.0(2) . . ?
C15 P1 Pd1 110.81(18) . 3_567 ?
C8 P1 Pd1 108.02(17) . 3_567 ?
C1 P1 Pd1 114.98(18) . 3_567 ?
S1 O1 Pd1 130.5(2) . . ?
S1 O3 Pd1 120.5(2) . 3_567 ?
S2 O4 Pd1 116.2(2) . 3_567 ?
C6 C1 C2 119.6(5) . . ?
C6 C1 P1 118.0(4) . . ?
C2 C1 P1 122.3(4) . . ?
C3 C2 C1 119.4(5) . . ?
C3 C2 S2 118.0(4) . . ?
C1 C2 S2 122.6(4) . . ?
C2 C3 C4 120.6(5) . . ?
C5 C4 C3 120.3(5) . . ?
C6 C5 C4 118.5(5) . . ?
C6 C5 C7 121.1(5) . . ?
C4 C5 C7 120.4(5) . . ?
C1 C6 C5 121.7(5) . . ?
C9 C8 C13 118.0(5) . . ?
C9 C8 P1 122.6(4) . . ?
C13 C8 P1 119.4(4) . . ?
C10 C9 C8 120.8(5) . . ?
C10 C9 S1 114.3(4) . . ?
C8 C9 S1 124.8(4) . . ?
C9 C10 C11 119.8(5) . . ?
C12 C11 C10 120.8(5) . . ?
C11 C12 C13 119.3(5) . . ?
C11 C12 C14 120.5(5) . . ?
C13 C12 C14 120.2(5) . . ?
C12 C13 C8 121.1(5) . . ?
C20 C15 C16 119.5(5) . . ?
C20 C15 P1 122.5(4) . . ?
C16 C15 P1 117.9(4) . . ?
C17 C16 C15 119.1(5) . . ?
C16 C17 C18 120.9(5) . . ?
C17 C18 C19 119.5(5) . . ?
C20 C19 C18 120.7(5) . . ?
C19 C20 C15 120.2(5) . . ?
Cl2 C21 Cl1 110.8(4) . . ?
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 O4 1.990(4) 3_567 ?
Pd1 O3 2.019(4) 3_567 ?
Pd1 O1 2.121(4) . ?
Pd1 P1 2.1638(16) 3_567 ?
S1 O2 1.410(4) . ?
S1 O1 1.460(4) . ?
S1 O3 1.489(4) . ?
S1 C9 1.779(5) . ?
S2 O6 1.416(4) . ?
S2 O5 1.434(4) . ?
S2 O4 1.511(4) . ?
S2 C2 1.762(5) . ?
P1 C15 1.784(5) . ?
P1 C8 1.804(5) . ?
P1 C1 1.811(5) . ?
P1 Pd1 2.1638(16) 3_567 ?
O3 Pd1 2.019(4) 3_567 ?
O4 Pd1 1.990(4) 3_567 ?
C1 C6 1.378(7) . ?
C1 C2 1.387(7) . ?
C2 C3 1.373(7) . ?
C3 C4 1.391(8) . ?
C4 C5 1.381(8) . ?
C5 C6 1.380(7) . ?
C5 C7 1.493(7) . ?
C8 C9 1.387(7) . ?
C8 C13 1.407(7) . ?
C9 C10 1.379(7) . ?
C10 C11 1.381(7) . ?
C11 C12 1.372(7) . ?
C12 C13 1.375(7) . ?
C12 C14 1.505(7) . ?
C15 C20 1.382(7) . ?
C15 C16 1.391(7) . ?
C16 C17 1.368(7) . ?
C17 C18 1.370(8) . ?
C18 C19 1.371(8) . ?
C19 C20 1.355(7) . ?
Cl1 C21 1.762(6) . ?
Cl2 C21 1.753(7) . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 S1 O1 Pd1 -75.0(3) . . . . ?
O3 S1 O1 Pd1 51.0(3) . . . . ?
C9 S1 O1 Pd1 167.3(3) . . . . ?
O4 Pd1 O1 S1 75.3(3) 3_567 . . . ?
O3 Pd1 O1 S1 -107.1(3) 3_567 . . . ?
O2 S1 O3 Pd1 -173.1(2) . . . 3_567 ?
O1 S1 O3 Pd1 58.0(3) . . . 3_567 ?
C9 S1 O3 Pd1 -55.3(3) . . . 3_567 ?
O6 S2 O4 Pd1 -166.6(2) . . . 3_567 ?
O5 S2 O4 Pd1 -35.4(3) . . . 3_567 ?
C2 S2 O4 Pd1 79.4(3) . . . 3_567 ?
C15 P1 C1 C6 -33.0(5) . . . . ?
C8 P1 C1 C6 82.4(4) . . . . ?
Pd1 P1 C1 C6 -155.5(3) 3_567 . . . ?
C15 P1 C1 C2 142.2(4) . . . . ?
C8 P1 C1 C2 -102.5(5) . . . . ?
Pd1 P1 C1 C2 19.7(5) 3_567 . . . ?
C6 C1 C2 C3 -1.2(8) . . . . ?
P1 C1 C2 C3 -176.3(4) . . . . ?
C6 C1 C2 S2 -179.5(4) . . . . ?
P1 C1 C2 S2 5.4(7) . . . . ?
O6 S2 C2 C3 10.7(5) . . . . ?
O5 S2 C2 C3 -115.4(4) . . . . ?
O4 S2 C2 C3 126.4(4) . . . . ?
O6 S2 C2 C1 -170.9(4) . . . . ?
O5 S2 C2 C1 62.9(5) . . . . ?
O4 S2 C2 C1 -55.2(5) . . . . ?
C1 C2 C3 C4 0.0(8) . . . . ?
S2 C2 C3 C4 178.4(4) . . . . ?
C2 C3 C4 C5 0.3(8) . . . . ?
C3 C4 C5 C6 0.5(8) . . . . ?
C3 C4 C5 C7 179.2(5) . . . . ?
C2 C1 C6 C5 2.1(8) . . . . ?
P1 C1 C6 C5 177.4(4) . . . . ?
C4 C5 C6 C1 -1.7(8) . . . . ?
C7 C5 C6 C1 179.6(5) . . . . ?
C15 P1 C8 C9 -84.8(4) . . . . ?
C1 P1 C8 C9 160.9(4) . . . . ?
Pd1 P1 C8 C9 34.6(4) 3_567 . . . ?
C15 P1 C8 C13 93.6(4) . . . . ?
C1 P1 C8 C13 -20.8(5) . . . . ?
Pd1 P1 C8 C13 -147.0(3) 3_567 . . . ?
C13 C8 C9 C10 2.7(7) . . . . ?
P1 C8 C9 C10 -178.9(4) . . . . ?
C13 C8 C9 S1 -174.0(4) . . . . ?
P1 C8 C9 S1 4.4(6) . . . . ?
O2 S1 C9 C10 -57.0(4) . . . . ?
O1 S1 C9 C10 65.7(4) . . . . ?
O3 S1 C9 C10 -176.1(4) . . . . ?
O2 S1 C9 C8 119.9(4) . . . . ?
O1 S1 C9 C8 -117.4(4) . . . . ?
O3 S1 C9 C8 0.7(5) . . . . ?
C8 C9 C10 C11 -2.3(8) . . . . ?
S1 C9 C10 C11 174.7(4) . . . . ?
C9 C10 C11 C12 -1.6(8) . . . . ?
C10 C11 C12 C13 5.0(8) . . . . ?
C10 C11 C12 C14 -173.9(5) . . . . ?
C11 C12 C13 C8 -4.6(8) . . . . ?
C14 C12 C13 C8 174.3(5) . . . . ?
C9 C8 C13 C12 0.8(7) . . . . ?
P1 C8 C13 C12 -177.6(4) . . . . ?
C8 P1 C15 C20 -8.1(5) . . . . ?
C1 P1 C15 C20 109.2(5) . . . . ?
Pd1 P1 C15 C20 -125.7(4) 3_567 . . . ?
C8 P1 C15 C16 173.9(4) . . . . ?
C1 P1 C15 C16 -68.8(5) . . . . ?
Pd1 P1 C15 C16 56.3(4) 3_567 . . . ?
C20 C15 C16 C17 0.2(8) . . . . ?
P1 C15 C16 C17 178.3(4) . . . . ?
C15 C16 C17 C18 -0.4(8) . . . . ?
C16 C17 C18 C19 -0.4(9) . . . . ?
C17 C18 C19 C20 1.4(9) . . . . ?
C18 C19 C20 C15 -1.6(8) . . . . ?
C16 C15 C20 C19 0.8(8) . . . . ?
P1 C15 C20 C19 -177.2(4) . . . . ?
