#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:01:21 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178709 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/20/4082060.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_4082060
loop_
_publ_author_name
'Lau, Ka-Cheong'
'Petro, Benjamin J.'
'Bontemps, Sébastien'
'Jordan, Richard F.'
_publ_section_title
;
 Comparative Reactivity of Zr-- and Pd--Alkyl Complexes with Carbon
 Dioxide
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6895
_journal_paper_doi               10.1021/om401082k
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C46 H84 Li2 O10 P2 Pd2 S2'
_chemical_formula_weight         1149.87
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_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                 117.41(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.064(5)
_cell_length_b                   17.858(8)
_cell_length_c                   14.970(5)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      1.91
_cell_volume                     2625.7(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1579
_diffrn_reflns_av_sigmaI/netI    0.2114
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25333
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.9021
_exptl_absorpt_correction_T_min  0.9021
_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    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.715
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.715
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0191P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                2246
_reflns_number_total             4651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401082k_si_002.cif
_cod_data_source_block           {[Li(THF)2][(PO-iPr)PdMe2]}2(3a)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4082060
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
C1 C 0.4422(7) 0.7096(4) 0.5064(5) 0.0284(19) Uani 1 1 d .
C2 C 0.5669(7) 0.7171(4) 0.5875(5) 0.033(2) Uani 1 1 d .
H2 H 0.6162 0.6747 0.6205 0.040 Uiso 1 1 calc R
C3 C 0.6204(7) 0.7881(4) 0.6209(5) 0.033(2) Uani 1 1 d .
H3 H 0.7062 0.7929 0.6758 0.039 Uiso 1 1 calc R
C4 C 0.5495(7) 0.8502(4) 0.5747(5) 0.0309(18) Uani 1 1 d .
C5 C 0.4232(7) 0.8403(4) 0.4916(5) 0.0317(19) Uani 1 1 d .
H5 H 0.3735 0.8830 0.4605 0.038 Uiso 1 1 calc R
C6 C 0.3661(7) 0.7717(4) 0.4516(5) 0.0244(18) Uani 1 1 d .
C7 C 0.6018(7) 0.9272(4) 0.6146(5) 0.043(2) Uani 1 1 d .
H7A H 0.6104 0.9322 0.6812 0.065 Uiso 1 1 calc R
H7B H 0.5392 0.9641 0.5713 0.065 Uiso 1 1 calc R
H7C H 0.6892 0.9344 0.6169 0.065 Uiso 1 1 calc R
C8 C 0.1042(6) 0.8378(4) 0.3649(5) 0.0324(19) Uani 1 1 d .
H8 H 0.1514 0.8859 0.3751 0.039 Uiso 1 1 calc R
C9 C 0.0937(7) 0.8182(4) 0.4605(5) 0.044(2) Uani 1 1 d .
H9A H 0.0375 0.8545 0.4710 0.066 Uiso 1 1 calc R
H9B H 0.1830 0.8185 0.5170 0.066 Uiso 1 1 calc R
H9C H 0.0542 0.7694 0.4536 0.066 Uiso 1 1 calc R
C10 C -0.0359(6) 0.8451(4) 0.2762(5) 0.042(2) Uani 1 1 d .
H10A H -0.0849 0.7991 0.2673 0.062 Uiso 1 1 calc R
H10B H -0.0274 0.8559 0.2166 0.062 Uiso 1 1 calc R
H10C H -0.0844 0.8850 0.2886 0.062 Uiso 1 1 calc R
C11 C 0.2374(7) 0.8036(4) 0.2399(5) 0.0299(19) Uani 1 1 d .
H11 H 0.1549 0.7953 0.1764 0.036 Uiso 1 1 calc R
C12 C 0.3505(7) 0.7574(4) 0.2336(5) 0.041(2) Uani 1 1 d .
H12A H 0.3605 0.7729 0.1760 0.061 Uiso 1 1 calc R
H12B H 0.3268 0.7052 0.2275 0.061 Uiso 1 1 calc R
H12C H 0.4347 0.7651 0.2935 0.061 Uiso 1 1 calc R
C13 C 0.2726(7) 0.8862(4) 0.2415(5) 0.040(2) Uani 1 1 d .
H13A H 0.3553 0.8968 0.3014 0.060 Uiso 1 1 calc R
H13B H 0.2001 0.9161 0.2408 0.060 Uiso 1 1 calc R
H13C H 0.2845 0.8977 0.1834 0.060 Uiso 1 1 calc R
C14 C -0.0260(6) 0.6737(3) 0.1561(4) 0.0324(19) Uani 1 1 d .
H14A H 0.0040 0.6484 0.1133 0.049 Uiso 1 1 calc R
H14B H -0.0265 0.7267 0.1458 0.049 Uiso 1 1 calc R
H14C H -0.1163 0.6573 0.1403 0.049 Uiso 1 1 calc R
C15 C 0.0116(6) 0.5466(3) 0.2663(5) 0.0318(19) Uani 1 1 d .
H15A H -0.0641 0.5456 0.2811 0.048 Uiso 1 1 calc R
H15B H 0.0773 0.5096 0.3062 0.048 Uiso 1 1 calc R
H15C H -0.0197 0.5360 0.1962 0.048 Uiso 1 1 calc R
C16 C 0.7020(7) 0.4607(4) 0.8426(5) 0.040(2) Uani 1 1 d .
H16A H 0.7550 0.4386 0.8127 0.048 Uiso 1 1 calc R
H16B H 0.6637 0.4207 0.8655 0.048 Uiso 1 1 calc R
C17 C 0.7900(7) 0.5112(4) 0.9291(6) 0.052(2) Uani 1 1 d .
H17A H 0.8001 0.4912 0.9924 0.062 Uiso 1 1 calc R
H17B H 0.8795 0.5172 0.9331 0.062 Uiso 1 1 calc R
C18 C 0.7152(7) 0.5834(4) 0.9050(5) 0.049(2) Uani 1 1 d .
H18A H 0.6552 0.5863 0.9359 0.059 Uiso 1 1 calc R
H18B H 0.7776 0.6254 0.9275 0.059 Uiso 1 1 calc R
C19 C 0.6377(7) 0.5819(4) 0.7956(5) 0.041(2) Uani 1 1 d .
H19A H 0.5596 0.6150 0.7727 0.049 Uiso 1 1 calc R
H19B H 0.6941 0.5974 0.7649 0.049 Uiso 1 1 calc R
C20 C 0.3206(7) 0.3489(4) 0.6170(6) 0.049(2) Uani 1 1 d .
H20A H 0.3798 0.3349 0.6862 0.059 Uiso 1 1 calc R
H20B H 0.3522 0.3241 0.5739 0.059 Uiso 1 1 calc R
C21 C 0.1757(7) 0.3273(4) 0.5876(6) 0.057(3) Uani 1 1 d .
H21A H 0.1537 0.2791 0.5539 0.068 Uiso 1 1 calc R
H21B H 0.1600 0.3249 0.6462 0.068 Uiso 1 1 calc R
C22 C 0.0939(7) 0.3874(4) 0.5188(5) 0.046(2) Uani 1 1 d .
H22A H 0.0747 0.3769 0.4500 0.055 Uiso 1 1 calc R
H22B H 0.0089 0.3949 0.5216 0.055 Uiso 1 1 calc R
C23 C 0.1845(7) 0.4525(4) 0.5592(6) 0.053(2) Uani 1 1 d .
H23A H 0.1699 0.4871 0.5053 0.063 Uiso 1 1 calc R
H23B H 0.1650 0.4784 0.6081 0.063 Uiso 1 1 calc R
Li1 Li 0.4868(12) 0.4775(7) 0.6301(9) 0.041(4) Uani 1 1 d .
O1 O 0.4636(4) 0.5727(2) 0.5662(3) 0.0358(13) Uani 1 1 d .
O2 O 0.2392(4) 0.6156(2) 0.4535(3) 0.0303(12) Uani 1 1 d .
O3 O 0.4027(4) 0.5941(2) 0.3913(3) 0.0339(13) Uani 1 1 d .
O4 O 0.5957(5) 0.5074(2) 0.7708(3) 0.0360(13) Uani 1 1 d .
O5 O 0.3199(5) 0.4276(3) 0.6051(4) 0.0410(14) Uani 1 1 d .
P1 P 0.20244(19) 0.76622(10) 0.33855(14) 0.0296(5) Uani 1 1 d .
Pd1 Pd 0.09952(6) 0.65002(3) 0.29895(4) 0.03104(18) Uani 1 1 d .
S1 S 0.3814(2) 0.61534(10) 0.47551(15) 0.0308(5) 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 0.0033 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'
Li Li -0.0003 0.0001 '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
C2 C1 C6 122.2(6) . .
C2 C1 S1 115.3(5) . .
C6 C1 S1 122.5(5) . .
C1 C2 C3 119.9(7) . .
C4 C3 C2 120.9(7) . .
C3 C4 C5 117.5(7) . .
C3 C4 C7 121.3(6) . .
C5 C4 C7 121.1(7) . .
C6 C5 C4 124.9(7) . .
C5 C6 C1 114.5(6) . .
C5 C6 P1 120.6(5) . .
C1 C6 P1 124.8(5) . .
C10 C8 C9 110.6(5) . .
C10 C8 P1 109.9(5) . .
C9 C8 P1 110.4(5) . .
C13 C11 C12 108.2(5) . .
C13 C11 P1 119.4(5) . .
C12 C11 P1 109.6(5) . .
O4 C16 C17 106.1(6) . .
C18 C17 C16 104.1(6) . .
C19 C18 C17 103.4(6) . .
O4 C19 C18 105.4(6) . .
O5 C20 C21 105.9(6) . .
C22 C21 C20 104.3(6) . .
C23 C22 C21 101.8(6) . .
O5 C23 C22 108.8(6) . .
O3 Li1 O1 117.7(6) 3_666 .
O3 Li1 O5 106.8(6) 3_666 .
O1 Li1 O5 114.8(7) . .
O3 Li1 O4 103.9(6) 3_666 .
O1 Li1 O4 99.8(6) . .
O5 Li1 O4 113.3(6) . .
S1 O1 Li1 144.8(5) . .
S1 O2 Pd1 113.8(3) . .
S1 O3 Li1 134.9(5) . 3_666
C19 O4 C16 107.2(5) . .
C19 O4 Li1 120.5(6) . .
C16 O4 Li1 122.1(5) . .
C23 O5 C20 108.6(5) . .
C23 O5 Li1 131.3(6) . .
C20 O5 Li1 119.1(6) . .
C11 P1 C6 104.0(3) . .
C11 P1 C8 106.7(3) . .
C6 P1 C8 101.4(3) . .
C11 P1 Pd1 112.7(2) . .
C6 P1 Pd1 116.6(2) . .
C8 P1 Pd1 114.2(2) . .
C14 Pd1 C15 85.1(2) . .
C14 Pd1 O2 175.9(2) . .
C15 Pd1 O2 91.5(2) . .
C14 Pd1 P1 95.92(19) . .
C15 Pd1 P1 178.94(19) . .
O2 Pd1 P1 87.52(12) . .
O3 S1 O2 113.6(3) . .
O3 S1 O1 113.4(3) . .
O2 S1 O1 111.1(3) . .
O3 S1 C1 106.3(3) . .
O2 S1 C1 107.1(3) . .
O1 S1 C1 104.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.361(8) .
C1 C6 1.405(8) .
C1 S1 1.793(7) .
C2 C3 1.393(8) .
C3 C4 1.351(9) .
C4 C5 1.390(8) .
C4 C7 1.505(8) .
C5 C6 1.382(8) .
C6 P1 1.825(7) .
C8 C10 1.512(8) .
C8 C9 1.529(8) .
C8 P1 1.835(6) .
C11 C13 1.522(8) .
C11 C12 1.538(8) .
C11 P1 1.818(7) .
C14 Pd1 1.986(6) .
C15 Pd1 2.038(6) .
C16 O4 1.438(7) .
C16 C17 1.509(8) .
C17 C18 1.484(9) .
C18 C19 1.458(9) .
C19 O4 1.402(7) .
C20 O5 1.416(8) .
C20 C21 1.504(8) .
C21 C22 1.474(9) .
C22 C23 1.471(9) .
C23 O5 1.403(7) .
Li1 O3 1.896(13) 3_666
Li1 O1 1.909(13) .
Li1 O5 1.926(13) .
Li1 O4 1.959(13) .
O1 S1 1.453(4) .
O2 S1 1.452(4) .
O2 Pd1 2.197(4) .
O3 S1 1.436(4) .
O3 Li1 1.896(13) 3_666
P1 Pd1 2.309(2) .
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 2.6(11) .
S1 C1 C2 C3 -176.8(5) .
C1 C2 C3 C4 0.9(11) .
C2 C3 C4 C5 -1.5(11) .
C2 C3 C4 C7 175.5(7) .
C3 C4 C5 C6 -1.3(11) .
C7 C4 C5 C6 -178.4(6) .
C4 C5 C6 C1 4.4(11) .
C4 C5 C6 P1 -177.3(5) .
C2 C1 C6 C5 -5.0(11) .
S1 C1 C6 C5 174.3(5) .
C2 C1 C6 P1 176.8(5) .
S1 C1 C6 P1 -3.9(9) .
O4 C16 C17 C18 6.9(8) .
C16 C17 C18 C19 -26.6(8) .
C17 C18 C19 O4 37.7(8) .
O5 C20 C21 C22 25.1(8) .
C20 C21 C22 C23 -31.9(8) .
C21 C22 C23 O5 28.7(8) .
O3 Li1 O1 S1 89.0(10) 3_666
O5 Li1 O1 S1 -38.0(12) .
O4 Li1 O1 S1 -159.5(6) .
C18 C19 O4 C16 -34.1(8) .
C18 C19 O4 Li1 180.0(6) .
C17 C16 O4 C19 16.5(8) .
C17 C16 O4 Li1 161.7(6) .
O3 Li1 O4 C19 118.8(6) 3_666
O1 Li1 O4 C19 -3.2(8) .
O5 Li1 O4 C19 -125.7(7) .
O3 Li1 O4 C16 -22.1(9) 3_666
O1 Li1 O4 C16 -144.0(6) .
O5 Li1 O4 C16 93.5(8) .
C22 C23 O5 C20 -13.5(8) .
C22 C23 O5 Li1 154.9(7) .
C21 C20 O5 C23 -7.4(8) .
C21 C20 O5 Li1 -177.5(6) .
O3 Li1 O5 C23 -142.1(7) 3_666
O1 Li1 O5 C23 -9.7(11) .
O4 Li1 O5 C23 104.1(8) .
O3 Li1 O5 C20 25.4(9) 3_666
O1 Li1 O5 C20 157.8(6) .
O4 Li1 O5 C20 -88.4(8) .
C13 C11 P1 C6 -67.5(6) .
C12 C11 P1 C6 58.0(5) .
C13 C11 P1 C8 39.1(6) .
C12 C11 P1 C8 164.7(5) .
C13 C11 P1 Pd1 165.3(5) .
C12 C11 P1 Pd1 -69.2(5) .
C5 C6 P1 C11 67.2(6) .
C1 C6 P1 C11 -114.6(6) .
C5 C6 P1 C8 -43.4(6) .
C1 C6 P1 C8 134.7(6) .
C5 C6 P1 Pd1 -168.0(5) .
C1 C6 P1 Pd1 10.1(7) .
C10 C8 P1 C11 68.7(5) .
C9 C8 P1 C11 -168.9(5) .
C10 C8 P1 C6 177.3(5) .
C9 C8 P1 C6 -60.4(5) .
C10 C8 P1 Pd1 -56.5(5) .
C9 C8 P1 Pd1 65.9(5) .
S1 O2 Pd1 C15 115.2(3) .
S1 O2 Pd1 P1 -64.5(2) .
C11 P1 Pd1 C14 -41.5(3) .
C6 P1 Pd1 C14 -161.7(3) .
C8 P1 Pd1 C14 80.5(3) .
C11 P1 Pd1 O2 136.2(3) .
C6 P1 Pd1 O2 16.0(3) .
C8 P1 Pd1 O2 -101.8(3) .
Li1 O3 S1 O2 -127.7(7) 3_666
Li1 O3 S1 O1 0.4(7) 3_666
Li1 O3 S1 C1 114.8(7) 3_666
Pd1 O2 S1 O3 -34.4(3) .
Pd1 O2 S1 O1 -163.6(2) .
Pd1 O2 S1 C1 82.7(3) .
Li1 O1 S1 O3 -72.8(9) .
Li1 O1 S1 O2 56.6(9) .
Li1 O1 S1 C1 171.9(8) .
C2 C1 S1 O3 -102.0(6) .
C6 C1 S1 O3 78.6(6) .
C2 C1 S1 O2 136.3(6) .
C6 C1 S1 O2 -43.1(7) .
C2 C1 S1 O1 18.2(6) .
C6 C1 S1 O1 -161.1(6) .
