#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:45:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179456 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/53/4335363.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_4335363
loop_
_publ_author_name
'Arvind K. Gupta'
'S. Arun Dixith Reddy'
'Ramamoorthy Boomishankar'
_publ_section_title
;
 Facile Formation of Stable Tris(imido)phosphate Trianions as Their Tri-
 and Hexanuclear Pd(II) Complexes in Protic Solvents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7608
_journal_page_last               7614
_journal_paper_doi               10.1021/ic400686e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C30 H68 N6 O14 P2 Pd6 S2'
_chemical_formula_weight         1501.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.349(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.812(3)
_cell_length_b                   9.7381(14)
_cell_length_c                   23.628(3)
_cell_measurement_reflns_used    2382
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.31
_cell_volume                     4926.7(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and 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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11489
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    2.355
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       prism
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4197
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0368P)²+17.4423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                3339
_reflns_number_total             4197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400686e_7b.cif
_cod_data_source_block           compound7b
_cod_database_code               4335363
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 1.107065(19) 0.35382(5) 0.80653(2) 0.01262(13) Uani 1 1 d . . .
Pd2 Pd 1.016430(19) 0.35051(6) 0.85308(2) 0.01348(13) Uani 1 1 d . . .
Pd3 Pd 0.94026(2) 0.09326(6) 0.77679(2) 0.01550(13) Uani 1 1 d . . .
P1 P 0.89257(7) 0.31506(19) 0.80714(7) 0.0132(4) Uani 1 1 d . . .
O11 O 0.85135(18) 0.3581(5) 0.83139(19) 0.0181(10) Uani 1 1 d . . .
O1 O 0.9100(2) -0.0216(6) 0.6941(2) 0.0291(12) Uani 1 1 d . . .
O2 O 0.9861(2) -0.0335(6) 0.6694(2) 0.0282(12) Uani 1 1 d . . .
O3 O 1.15981(19) 0.2579(6) 0.89522(19) 0.0240(11) Uani 1 1 d . . .
O4 O 1.08995(18) 0.2508(6) 0.92883(19) 0.0236(11) Uani 1 1 d . . .
O5 O 1.07155(18) 0.4941(5) 0.84348(19) 0.0158(10) Uani 1 1 d D . .
H5 H 1.103(3) 0.469(10) 0.882(2) 0.06(3) Uiso 1 1 d D . .
C1 C 0.9342(3) -0.0633(7) 0.6622(3) 0.0172(14) Uani 1 1 d . . .
C2 C 0.8965(3) -0.1664(9) 0.6088(3) 0.0329(19) Uani 1 1 d . . .
H2A H 0.8567 -0.1831 0.6069 0.049 Uiso 1 1 calc R . .
H2B H 0.9199 -0.2526 0.6184 0.049 Uiso 1 1 calc R . .
H2C H 0.8886 -0.1303 0.5666 0.049 Uiso 1 1 calc R . .
C3 C 1.1426(3) 0.2246(8) 0.9350(3) 0.0190(15) Uani 1 1 d . . .
C4 C 1.1873(3) 0.1455(9) 0.9953(3) 0.0285(18) Uani 1 1 d . . .
H4A H 1.1679 0.1269 1.0217 0.043 Uiso 1 1 calc R . .
H4B H 1.2254 0.1996 1.0211 0.043 Uiso 1 1 calc R . .
H4C H 1.1978 0.0585 0.9824 0.043 Uiso 1 1 calc R . .
N1 N 0.8644(2) 0.2205(6) 0.7382(2) 0.0145(12) Uani 1 1 d . . .
C11 C 0.8003(3) 0.1631(7) 0.7004(3) 0.0156(14) Uani 1 1 d . . .
H11 H 0.7963 0.1192 0.6602 0.019 Uiso 1 1 calc R . .
C12 C 0.7518(3) 0.2768(8) 0.6777(3) 0.0230(17) Uani 1 1 d . . .
H12A H 0.7607 0.3456 0.6531 0.035 Uiso 1 1 calc R . .
H12B H 0.7534 0.3202 0.7159 0.035 Uiso 1 1 calc R . .
H12C H 0.7102 0.2379 0.6493 0.035 Uiso 1 1 calc R . .
C13 C 0.7896(3) 0.0514(8) 0.7386(3) 0.0248(16) Uani 1 1 d . . .
H13A H 0.8218 -0.0193 0.7518 0.037 Uiso 1 1 calc R . .
H13B H 0.7484 0.0102 0.7109 0.037 Uiso 1 1 calc R . .
H13C H 0.7917 0.0915 0.7777 0.037 Uiso 1 1 calc R . .
N2 N 0.9307(2) 0.4325(6) 0.7868(2) 0.0124(11) Uani 1 1 d . . .
C21 C 0.9259(3) 0.5859(8) 0.7900(3) 0.0181(14) Uani 1 1 d . . .
H21 H 0.9543 0.6268 0.7760 0.022 Uiso 1 1 calc R . .
C22 C 0.9484(3) 0.6358(8) 0.8590(3) 0.0264(17) Uani 1 1 d . . .
H22A H 0.9907 0.6011 0.8884 0.040 Uiso 1 1 calc R . .
H22B H 0.9202 0.6022 0.8737 0.040 Uiso 1 1 calc R . .
H22C H 0.9489 0.7364 0.8597 0.040 Uiso 1 1 calc R . .
C23 C 0.8603(3) 0.6382(8) 0.7424(3) 0.0271(17) Uani 1 1 d . . .
H23A H 0.8469 0.6043 0.6982 0.041 Uiso 1 1 calc R . .
H23B H 0.8603 0.7388 0.7423 0.041 Uiso 1 1 calc R . .
H23C H 0.8314 0.6050 0.7563 0.041 Uiso 1 1 calc R . .
N3 N 0.9550(2) 0.2147(6) 0.8537(2) 0.0159(12) Uani 1 1 d . . .
C31 C 0.9696(3) 0.1490(8) 0.9169(3) 0.0209(16) Uani 1 1 d . . .
H31 H 1.0087 0.0943 0.9325 0.025 Uiso 1 1 calc R . .
C32 C 0.9826(3) 0.2565(9) 0.9688(3) 0.0306(19) Uani 1 1 d . . .
H32A H 1.0159 0.3180 0.9734 0.046 Uiso 1 1 calc R . .
H32B H 0.9958 0.2111 1.0109 0.046 Uiso 1 1 calc R . .
H32C H 0.9446 0.3099 0.9558 0.046 Uiso 1 1 calc R . .
C33 C 0.9183(3) 0.0493(9) 0.9080(3) 0.0304(19) Uani 1 1 d . . .
H33A H 0.9113 -0.0186 0.8744 0.046 Uiso 1 1 calc R . .
H33B H 0.8796 0.1003 0.8944 0.046 Uiso 1 1 calc R . .
H33C H 0.9311 0.0023 0.9496 0.046 Uiso 1 1 calc R . .
S1 S 0.16298(13) 0.6190(4) 0.01639(14) 0.0264(10) Uiso 0.588(6) 1 d PDU A 1
C41 C 0.2145(6) 0.7214(17) 0.0687(7) 0.041(4) Uiso 0.588(6) 1 d PDU A 1
H41A H 0.2229 0.7942 0.0455 0.061 Uiso 0.588(6) 1 calc PR A 1
H41B H 0.2531 0.6704 0.0967 0.061 Uiso 0.588(6) 1 calc PR A 1
H41C H 0.1991 0.7622 0.0957 0.061 Uiso 0.588(6) 1 calc PR A 1
C42 C 0.1441(9) 0.4883(17) 0.0446(9) 0.047(6) Uiso 0.588(6) 1 d PDU A 1
H42A H 0.1130 0.4328 0.0080 0.070 Uiso 0.588(6) 1 calc PR A 1
H42B H 0.1264 0.5202 0.0712 0.070 Uiso 0.588(6) 1 calc PR A 1
H42C H 0.1813 0.4326 0.0718 0.070 Uiso 0.588(6) 1 calc PR A 1
O43 O 0.1785(6) 0.5631(14) -0.0345(4) 0.021(4) Uiso 0.588(6) 1 d PDU A 1
S1' S 0.20788(18) 0.5609(5) 0.03734(19) 0.0225(14) Uiso 0.412(6) 1 d PDU A 2
C41' C 0.2352(8) 0.6904(18) 0.0849(8) 0.026(4) Uiso 0.412(6) 1 d PDU A 2
H41D H 0.2629 0.7423 0.0744 0.039 Uiso 0.412(6) 1 calc PR A 2
H41E H 0.2588 0.6590 0.1305 0.039 Uiso 0.412(6) 1 calc PR A 2
H41F H 0.2007 0.7493 0.0789 0.039 Uiso 0.412(6) 1 calc PR A 2
C42' C 0.1609(10) 0.473(2) 0.0545(11) 0.030(6) Uiso 0.412(6) 1 d PDU A 2
H42D H 0.1437 0.3946 0.0248 0.045 Uiso 0.412(6) 1 calc PR A 2
H42E H 0.1267 0.5328 0.0490 0.045 Uiso 0.412(6) 1 calc PR A 2
H42F H 0.1844 0.4408 0.1000 0.045 Uiso 0.412(6) 1 calc PR A 2
O43' O 0.1890(8) 0.580(2) -0.0329(6) 0.027(6) Uiso 0.412(6) 1 d PDU A 2
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'
N N 0.0061 0.0033 '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'
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
N1 Pd1 O5 174.69(17) 2_756 .
N1 Pd1 O3 91.74(19) 2_756 .
O5 Pd1 O3 93.35(17) . .
N1 Pd1 N2 76.6(2) 2_756 2_756
O5 Pd1 N2 98.46(18) . 2_756
O3 Pd1 N2 166.92(17) . 2_756
N1 Pd1 P1 38.22(15) 2_756 2_756
O5 Pd1 P1 137.07(12) . 2_756
O3 Pd1 P1 128.88(13) . 2_756
N2 Pd1 P1 38.75(14) 2_756 2_756
N1 Pd1 Pd2 136.21(15) 2_756 .
O5 Pd1 Pd2 43.69(12) . .
O3 Pd1 Pd2 80.09(11) . .
N2 Pd1 Pd2 112.43(12) 2_756 .
P1 Pd1 Pd2 138.44(4) 2_756 .
N1 Pd1 Pd3 41.43(14) 2_756 2_756
O5 Pd1 Pd3 136.12(12) . 2_756
O3 Pd1 Pd3 96.83(15) . 2_756
N2 Pd1 Pd3 78.49(15) 2_756 2_756
P1 Pd1 Pd3 55.97(4) 2_756 2_756
Pd2 Pd1 Pd3 96.511(19) . 2_756
N1 Pd1 H5 161.0(10) 2_756 .
O5 Pd1 H5 24.3(9) . .
O3 Pd1 H5 70.2(14) . .
N2 Pd1 H5 120.6(16) 2_756 .
P1 Pd1 H5 156(2) 2_756 .
Pd2 Pd1 H5 48(2) . .
Pd3 Pd1 H5 143(3) 2_756 .
N3 Pd2 O4 91.46(19) . .
N3 Pd2 O5 174.29(17) . .
O4 Pd2 O5 94.07(18) . .
N3 Pd2 N2 76.5(2) . .
O4 Pd2 N2 166.31(17) . .
O5 Pd2 N2 98.14(18) . .
N3 Pd2 P1 38.29(14) . .
O4 Pd2 P1 128.25(13) . .
O5 Pd2 P1 136.65(12) . .
N2 Pd2 P1 38.79(14) . .
N3 Pd2 Pd1 136.58(15) . .
O4 Pd2 Pd1 79.69(11) . .
O5 Pd2 Pd1 43.63(12) . .
N2 Pd2 Pd1 113.53(12) . .
P1 Pd2 Pd1 140.50(4) . .
N3 Pd2 Pd3 40.36(14) . .
O4 Pd2 Pd3 97.89(16) . .
O5 Pd2 Pd3 136.98(11) . .
N2 Pd2 Pd3 77.28(15) . .
P1 Pd2 Pd3 55.37(4) . .
Pd1 Pd2 Pd3 98.440(19) . .
O2 Pd3 O1 92.6(2) 2_756 .
O2 Pd3 N3 95.5(2) 2_756 .
O1 Pd3 N3 170.30(18) . .
O2 Pd3 N1 169.01(17) 2_756 .
O1 Pd3 N1 95.4(2) . .
N3 Pd3 N1 75.87(19) . .
O2 Pd3 P1 133.55(14) 2_756 .
O1 Pd3 P1 133.50(15) . .
N3 Pd3 P1 38.09(14) . .
N1 Pd3 P1 38.08(14) . .
O2 Pd3 Pd1 146.93(13) 2_756 2_756
O1 Pd3 Pd1 90.16(16) . 2_756
N3 Pd3 Pd1 86.00(15) . 2_756
N1 Pd3 Pd1 40.74(14) . 2_756
P1 Pd3 Pd1 55.66(4) . 2_756
O2 Pd3 Pd2 92.07(16) 2_756 .
O1 Pd3 Pd2 145.16(14) . .
N3 Pd3 Pd2 39.95(14) . .
N1 Pd3 Pd2 85.59(15) . .
P1 Pd3 Pd2 55.00(4) . .
Pd1 Pd3 Pd2 68.147(19) 2_756 .
O11 P1 N1 120.3(2) . .
O11 P1 N3 120.2(2) . .
N1 P1 N3 96.3(3) . .
O11 P1 N2 121.1(3) . .
N1 P1 N2 96.4(2) . .
N3 P1 N2 96.6(2) . .
O11 P1 Pd2 132.91(19) . .
N1 P1 Pd2 106.78(16) . .
N3 P1 Pd2 48.07(19) . .
N2 P1 Pd2 49.36(16) . .
O11 P1 Pd1 134.38(19) . 2_756
N1 P1 Pd1 47.71(18) . 2_756
N3 P1 Pd1 105.37(16) . 2_756
N2 P1 Pd1 49.22(16) . 2_756
Pd2 P1 Pd1 78.99(4) . 2_756
O11 P1 Pd3 144.3(2) . .
N1 P1 Pd3 48.40(17) . .
N3 P1 Pd3 48.33(18) . .
N2 P1 Pd3 94.63(18) . .
Pd2 P1 Pd3 69.63(4) . .
Pd1 P1 Pd3 68.37(4) 2_756 .
C1 O1 Pd3 134.6(4) . .
C1 O2 Pd3 140.2(4) . 2_756
C3 O3 Pd1 126.8(4) . .
C3 O4 Pd2 127.6(4) . .
Pd1 O5 Pd2 92.7(2) . .
Pd1 O5 H5 85(6) . .
Pd2 O5 H5 89(6) . .
O2 C1 O1 128.5(6) . .
O2 C1 C2 115.5(6) . .
O1 C1 C2 115.9(5) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
O3 C3 O4 125.7(6) . .
O3 C3 C4 118.3(5) . .
O4 C3 C4 116.0(5) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C11 N1 P1 125.6(4) . .
C11 N1 Pd1 118.7(4) . 2_756
P1 N1 Pd1 94.1(3) . 2_756
C11 N1 Pd3 120.4(4) . .
P1 N1 Pd3 93.5(2) . .
Pd1 N1 Pd3 97.83(18) 2_756 .
N1 C11 C12 110.8(6) . .
N1 C11 C13 111.6(5) . .
C12 C11 C13 112.7(5) . .
N1 C11 H11 107.1 . .
C12 C11 H11 107.1 . .
C13 C11 H11 107.1 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C21 N2 P1 125.8(4) . .
C21 N2 Pd1 114.8(4) . 2_756
P1 N2 Pd1 92.0(2) . 2_756
C21 N2 Pd2 115.1(4) . .
P1 N2 Pd2 91.9(2) . .
Pd1 N2 Pd2 114.0(2) 2_756 .
N2 C21 C22 112.2(5) . .
N2 C21 C23 112.1(5) . .
C22 C21 C23 111.2(5) . .
N2 C21 H21 107.0 . .
C22 C21 H21 107.0 . .
C23 C21 H21 107.0 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C31 N3 P1 125.6(4) . .
C31 N3 Pd2 119.0(4) . .
P1 N3 Pd2 93.6(3) . .
C31 N3 Pd3 119.1(5) . .
P1 N3 Pd3 93.6(2) . .
Pd2 N3 Pd3 99.69(19) . .
N3 C31 C32 111.0(6) . .
N3 C31 C33 111.8(5) . .
C32 C31 C33 111.8(5) . .
N3 C31 H31 107.4 . .
C32 C31 H31 107.4 . .
C33 C31 H31 107.4 . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C31 C33 H33A 109.5 . .
C31 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C31 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
O43 S1 C41 114.0(7) . .
O43 S1 C42 106.6(8) . .
C41 S1 C42 117.3(8) . .
S1 C41 H41A 109.5 . .
S1 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
S1 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
S1 C42 H42A 109.5 . .
S1 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
S1 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
O43' S1' C41' 118.1(10) . .
O43' S1' C42' 118.2(10) . .
C41' S1' C42' 109.7(10) . .
S1' C41' H41D 109.5 . .
S1' C41' H41E 109.5 . .
H41D C41' H41E 109.5 . .
S1' C41' H41F 109.5 . .
H41D C41' H41F 109.5 . .
H41E C41' H41F 109.5 . .
S1' C42' H42D 109.5 . .
S1' C42' H42E 109.5 . .
H42D C42' H42E 109.5 . .
S1' C42' H42F 109.5 . .
H42D C42' H42F 109.5 . .
H42E C42' H42F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.015(5) 2_756
Pd1 O5 2.045(4) .
Pd1 O3 2.051(4) .
Pd1 N2 2.059(5) 2_756
Pd1 P1 2.7169(15) 2_756
Pd1 Pd2 2.9609(6) .
Pd1 Pd3 3.0588(8) 2_756
Pd1 H5 2.15(9) .
Pd2 N3 2.024(5) .
Pd2 O4 2.043(4) .
Pd2 O5 2.047(4) .
Pd2 N2 2.061(5) .
Pd2 P1 2.7151(15) .
Pd2 Pd3 3.1071(8) .
Pd3 O2 2.032(4) 2_756
Pd3 O1 2.036(4) .
Pd3 N3 2.041(5) .
Pd3 N1 2.043(5) .
Pd3 P1 2.7272(18) .
Pd3 Pd1 3.0588(8) 2_756
P1 O11 1.463(4) .
P1 N1 1.685(5) .
P1 N3 1.686(5) .
P1 N2 1.702(5) .
P1 Pd1 2.7170(15) 2_756
O1 C1 1.247(7) .
O2 C1 1.245(7) .
O2 Pd3 2.032(4) 2_756
O3 C3 1.257(7) .
O4 C3 1.264(7) .
O5 H5 0.89(2) .
C1 C2 1.510(10) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.502(9) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
N1 C11 1.485(7) .
N1 Pd1 2.015(5) 2_756
C11 C12 1.519(9) .
C11 C13 1.520(9) .
C11 H11 1.0000 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
N2 C21 1.503(9) .
N2 Pd1 2.059(5) 2_756
C21 C22 1.513(8) .
C21 C23 1.525(8) .
C21 H21 1.0000 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
N3 C31 1.491(7) .
C31 C32 1.519(10) .
C31 C33 1.529(10) .
C31 H31 1.0000 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
S1 O43 1.536(9) .
S1 C41 1.599(11) .
S1 C42 1.613(12) .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
S1' O43' 1.490(12) .
S1' C41' 1.594(13) .
S1' C42' 1.653(13) .
C41' H41D 0.9800 .
C41' H41E 0.9800 .
C41' H41F 0.9800 .
C42' H42D 0.9800 .
C42' H42E 0.9800 .
C42' H42F 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O43 0.89(2) 2.12(7) 2.840(11) 138(9) 1_656
O5 H5 O43' 0.89(2) 2.32(8) 3.019(16) 135(9) 1_656
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_4
N1 Pd1 Pd2 N3 -0.6(3) 2_756 .
O5 Pd1 Pd2 N3 171.7(3) . .
O3 Pd1 Pd2 N3 -82.7(2) . .
N2 Pd1 Pd2 N3 93.3(3) 2_756 .
P1 Pd1 Pd2 N3 57.1(2) 2_756 .
Pd3 Pd1 Pd2 N3 13.1(2) 2_756 .
N1 Pd1 Pd2 O4 80.5(2) 2_756 .
O5 Pd1 Pd2 O4 -107.2(2) . .
O3 Pd1 Pd2 O4 -1.6(2) . .
N2 Pd1 Pd2 O4 174.5(2) 2_756 .
P1 Pd1 Pd2 O4 138.18(17) 2_756 .
Pd3 Pd1 Pd2 O4 94.25(16) 2_756 .
N1 Pd1 Pd2 O5 -172.3(2) 2_756 .
O3 Pd1 Pd2 O5 105.6(2) . .
N2 Pd1 Pd2 O5 -78.4(2) 2_756 .
P1 Pd1 Pd2 O5 -114.64(17) 2_756 .
Pd3 Pd1 Pd2 O5 -158.57(16) 2_756 .
N1 Pd1 Pd2 N2 -95.8(3) 2_756 .
O5 Pd1 Pd2 N2 76.5(2) . .
O3 Pd1 Pd2 N2 -177.9(2) . .
N2 Pd1 Pd2 N2 -1.83(12) 2_756 .
P1 Pd1 Pd2 N2 -38.11(18) 2_756 .
Pd3 Pd1 Pd2 N2 -82.04(17) 2_756 .
N1 Pd1 Pd2 P1 -59.7(2) 2_756 .
O5 Pd1 Pd2 P1 112.60(17) . .
O3 Pd1 Pd2 P1 -141.81(17) . .
N2 Pd1 Pd2 P1 34.23(18) 2_756 .
P1 Pd1 Pd2 P1 -2.05(6) 2_756 .
Pd3 Pd1 Pd2 P1 -45.98(7) 2_756 .
N1 Pd1 Pd2 Pd3 -16.04(19) 2_756 .
O5 Pd1 Pd2 Pd3 156.27(16) . .
O3 Pd1 Pd2 Pd3 -98.13(15) . .
N2 Pd1 Pd2 Pd3 77.91(17) 2_756 .
P1 Pd1 Pd2 Pd3 41.63(7) 2_756 .
Pd3 Pd1 Pd2 Pd3 -2.30(2) 2_756 .
N3 Pd2 Pd3 O2 -96.1(2) . 2_756
O4 Pd2 Pd3 O2 -13.13(16) . 2_756
O5 Pd2 Pd3 O2 91.6(2) . 2_756
N2 Pd2 Pd3 O2 179.89(17) . 2_756
P1 Pd2 Pd3 O2 -144.72(12) . 2_756
Pd1 Pd2 Pd3 O2 67.54(11) . 2_756
N3 Pd2 Pd3 O1 166.4(3) . .
O4 Pd2 Pd3 O1 -110.7(3) . .
O5 Pd2 Pd3 O1 -6.0(3) . .
N2 Pd2 Pd3 O1 82.3(3) . .
P1 Pd2 Pd3 O1 117.7(3) . .
Pd1 Pd2 Pd3 O1 -30.0(3) . .
O4 Pd2 Pd3 N3 82.9(2) . .
O5 Pd2 Pd3 N3 -172.4(3) . .
N2 Pd2 Pd3 N3 -84.1(2) . .
P1 Pd2 Pd3 N3 -48.7(2) . .
Pd1 Pd2 Pd3 N3 163.6(2) . .
N3 Pd2 Pd3 N1 73.2(3) . .
O4 Pd2 Pd3 N1 156.11(17) . .
O5 Pd2 Pd3 N1 -99.2(2) . .
N2 Pd2 Pd3 N1 -10.87(18) . .
P1 Pd2 Pd3 N1 24.52(13) . .
Pd1 Pd2 Pd3 N1 -123.22(13) . .
N3 Pd2 Pd3 P1 48.7(2) . .
O4 Pd2 Pd3 P1 131.59(12) . .
O5 Pd2 Pd3 P1 -123.72(18) . .
N2 Pd2 Pd3 P1 -35.39(13) . .
Pd1 Pd2 Pd3 P1 -147.73(4) . .
N3 Pd2 Pd3 Pd1 111.2(2) . 2_756
O4 Pd2 Pd3 Pd1 -165.87(11) . 2_756
O5 Pd2 Pd3 Pd1 -61.19(17) . 2_756
N2 Pd2 Pd3 Pd1 27.15(12) . 2_756
P1 Pd2 Pd3 Pd1 62.54(4) . 2_756
Pd1 Pd2 Pd3 Pd1 -85.199(18) . 2_756
N3 Pd2 P1 O11 95.1(4) . .
O4 Pd2 P1 O11 76.2(3) . .
O5 Pd2 P1 O11 -88.9(3) . .
N2 Pd2 P1 O11 -97.6(4) . .
Pd1 Pd2 P1 O11 -157.1(3) . .
Pd3 Pd2 P1 O11 146.8(3) . .
N3 Pd2 P1 N1 -83.3(3) . .
O4 Pd2 P1 N1 -102.2(3) . .
O5 Pd2 P1 N1 92.6(3) . .
N2 Pd2 P1 N1 84.0(3) . .
Pd1 Pd2 P1 N1 24.5(2) . .
Pd3 Pd2 P1 N1 -31.6(2) . .
O4 Pd2 P1 N3 -18.9(3) . .
O5 Pd2 P1 N3 176.0(3) . .
N2 Pd2 P1 N3 167.3(3) . .
Pd1 Pd2 P1 N3 107.8(2) . .
Pd3 Pd2 P1 N3 51.7(2) . .
N3 Pd2 P1 N2 -167.3(3) . .
O4 Pd2 P1 N2 173.8(3) . .
O5 Pd2 P1 N2 8.6(3) . .
Pd1 Pd2 P1 N2 -59.5(2) . .
Pd3 Pd2 P1 N2 -115.6(2) . .
N3 Pd2 P1 Pd1 -122.5(2) . 2_756
O4 Pd2 P1 Pd1 -141.44(18) . 2_756
O5 Pd2 P1 Pd1 53.41(18) . 2_756
N2 Pd2 P1 Pd1 44.8(2) . 2_756
Pd1 Pd2 P1 Pd1 -14.71(8) . 2_756
Pd3 Pd2 P1 Pd1 -70.83(3) . 2_756
N3 Pd2 P1 Pd3 -51.7(2) . .
O4 Pd2 P1 Pd3 -70.61(19) . .
O5 Pd2 P1 Pd3 124.25(17) . .
N2 Pd2 P1 Pd3 115.6(2) . .
Pd1 Pd2 P1 Pd3 56.12(7) . .
O2 Pd3 P1 O11 -83.9(4) 2_756 .
O1 Pd3 P1 O11 87.5(4) . .
N3 Pd3 P1 O11 -85.2(4) . .
N1 Pd3 P1 O11 85.5(4) . .
Pd1 Pd3 P1 O11 137.5(3) 2_756 .
Pd2 Pd3 P1 O11 -136.7(3) . .
O2 Pd3 P1 N1 -169.4(3) 2_756 .
O1 Pd3 P1 N1 2.1(3) . .
N3 Pd3 P1 N1 -170.7(3) . .
Pd1 Pd3 P1 N1 52.0(2) 2_756 .
Pd2 Pd3 P1 N1 137.9(2) . .
O2 Pd3 P1 N3 1.4(3) 2_756 .
O1 Pd3 P1 N3 172.8(3) . .
N1 Pd3 P1 N3 170.7(3) . .
Pd1 Pd3 P1 N3 -137.3(2) 2_756 .
Pd2 Pd3 P1 N3 -51.4(2) . .
O2 Pd3 P1 N2 96.1(2) 2_756 .
O1 Pd3 P1 N2 -92.4(2) . .
N3 Pd3 P1 N2 94.8(3) . .
N1 Pd3 P1 N2 -94.5(3) . .
Pd1 Pd3 P1 N2 -42.52(16) 2_756 .
Pd2 Pd3 P1 N2 43.35(16) . .
O2 Pd3 P1 Pd2 52.79(19) 2_756 .
O1 Pd3 P1 Pd2 -135.80(19) . .
N3 Pd3 P1 Pd2 51.4(2) . .
N1 Pd3 P1 Pd2 -137.9(2) . .
Pd1 Pd3 P1 Pd2 -85.87(4) 2_756 .
O2 Pd3 P1 Pd1 138.66(19) 2_756 2_756
O1 Pd3 P1 Pd1 -49.93(19) . 2_756
N3 Pd3 P1 Pd1 137.3(2) . 2_756
N1 Pd3 P1 Pd1 -52.0(2) . 2_756
Pd2 Pd3 P1 Pd1 85.87(4) . 2_756
O2 Pd3 O1 C1 -55.1(7) 2_756 .
N3 Pd3 O1 C1 158.5(11) . .
N1 Pd3 O1 C1 132.4(7) . .
P1 Pd3 O1 C1 131.1(6) . .
Pd1 Pd3 O1 C1 91.9(7) 2_756 .
Pd2 Pd3 O1 C1 42.3(8) . .
N1 Pd1 O3 C3 -133.5(6) 2_756 .
O5 Pd1 O3 C3 45.0(6) . .
N2 Pd1 O3 C3 -160.4(8) 2_756 .
P1 Pd1 O3 C3 -143.4(5) 2_756 .
Pd2 Pd1 O3 C3 3.2(6) . .
Pd3 Pd1 O3 C3 -92.2(6) 2_756 .
N3 Pd2 O4 C3 138.1(6) . .
O5 Pd2 O4 C3 -40.5(6) . .
N2 Pd2 O4 C3 166.3(8) . .
P1 Pd2 O4 C3 149.7(5) . .
Pd1 Pd2 O4 C3 0.9(6) . .
Pd3 Pd2 O4 C3 98.1(6) . .
N1 Pd1 O5 Pd2 92(2) 2_756 .
O3 Pd1 O5 Pd2 -71.88(18) . .
N2 Pd1 O5 Pd2 113.75(17) 2_756 .
P1 Pd1 O5 Pd2 117.72(15) 2_756 .
Pd3 Pd1 O5 Pd2 31.6(2) 2_756 .
N3 Pd2 O5 Pd1 -95.1(19) . .
O4 Pd2 O5 Pd1 70.45(18) . .
N2 Pd2 O5 Pd1 -115.74(17) . .
P1 Pd2 O5 Pd1 -121.20(14) . .
Pd3 Pd2 O5 Pd1 -35.7(2) . .
Pd3 O2 C1 O1 -5.3(13) 2_756 .
Pd3 O2 C1 C2 176.5(5) 2_756 .
Pd3 O1 C1 O2 -7.6(12) . .
Pd3 O1 C1 C2 170.5(5) . .
Pd1 O3 C3 O4 -3.8(11) . .
Pd1 O3 C3 C4 175.6(5) . .
Pd2 O4 C3 O3 1.2(11) . .
Pd2 O4 C3 C4 -178.2(5) . .
O11 P1 N1 C11 -5.7(6) . .
N3 P1 N1 C11 124.9(5) . .
N2 P1 N1 C11 -137.7(5) . .
Pd2 P1 N1 C11 172.9(5) . .
Pd1 P1 N1 C11 -130.0(6) 2_756 .
Pd3 P1 N1 C11 131.9(6) . .
O11 P1 N1 Pd1 124.3(3) . 2_756
N3 P1 N1 Pd1 -105.1(2) . 2_756
N2 P1 N1 Pd1 -7.6(2) . 2_756
Pd2 P1 N1 Pd1 -57.0(2) . 2_756
Pd3 P1 N1 Pd1 -98.1(2) . 2_756
O11 P1 N1 Pd3 -137.6(3) . .
N3 P1 N1 Pd3 -7.0(2) . .
N2 P1 N1 Pd3 90.5(2) . .
Pd2 P1 N1 Pd3 41.1(2) . .
Pd1 P1 N1 Pd3 98.1(2) 2_756 .
O2 Pd3 N1 C11 -90.8(12) 2_756 .
O1 Pd3 N1 C11 46.1(4) . .
N3 Pd3 N1 C11 -129.5(4) . .
P1 Pd3 N1 C11 -135.4(5) . .
Pd1 Pd3 N1 C11 130.0(5) 2_756 .
Pd2 Pd3 N1 C11 -168.9(4) . .
O2 Pd3 N1 P1 44.6(12) 2_756 .
O1 Pd3 N1 P1 -178.5(2) . .
N3 Pd3 N1 P1 5.9(2) . .
Pd1 Pd3 N1 P1 -94.6(3) 2_756 .
Pd2 Pd3 N1 P1 -33.45(18) . .
O2 Pd3 N1 Pd1 139.2(10) 2_756 2_756
O1 Pd3 N1 Pd1 -83.9(2) . 2_756
N3 Pd3 N1 Pd1 100.5(2) . 2_756
P1 Pd3 N1 Pd1 94.6(3) . 2_756
Pd2 Pd3 N1 Pd1 61.15(16) . 2_756
P1 N1 C11 C12 58.6(7) . .
Pd1 N1 C11 C12 -60.8(6) 2_756 .
Pd3 N1 C11 C12 179.1(4) . .
P1 N1 C11 C13 -67.8(7) . .
Pd1 N1 C11 C13 172.7(4) 2_756 .
Pd3 N1 C11 C13 52.7(6) . .
O11 P1 N2 C21 -1.1(6) . .
N1 P1 N2 C21 130.3(5) . .
N3 P1 N2 C21 -132.5(5) . .
Pd2 P1 N2 C21 -123.1(5) . .
Pd1 P1 N2 C21 122.8(5) 2_756 .
Pd3 P1 N2 C21 178.9(4) . .
O11 P1 N2 Pd1 -123.9(2) . 2_756
N1 P1 N2 Pd1 7.5(2) . 2_756
N3 P1 N2 Pd1 104.6(2) . 2_756
Pd2 P1 N2 Pd1 114.1(2) . 2_756
Pd3 P1 N2 Pd1 56.07(15) . 2_756
O11 P1 N2 Pd2 122.0(2) . .
N1 P1 N2 Pd2 -106.6(2) . .
N3 P1 N2 Pd2 -9.5(2) . .
Pd1 P1 N2 Pd2 -114.1(2) 2_756 .
Pd3 P1 N2 Pd2 -58.01(15) . .
N3 Pd2 N2 C21 139.4(4) . .
O4 Pd2 N2 C21 110.3(9) . .
O5 Pd2 N2 C21 -42.7(4) . .
P1 Pd2 N2 C21 131.3(5) . .
Pd1 Pd2 N2 C21 -85.4(4) . .
Pd3 Pd2 N2 C21 -179.1(4) . .
N3 Pd2 N2 P1 8.0(2) . .
O4 Pd2 N2 P1 -21.1(10) . .
O5 Pd2 N2 P1 -174.0(2) . .
Pd1 Pd2 N2 P1 143.30(13) . .
Pd3 Pd2 N2 P1 49.52(16) . .
N3 Pd2 N2 Pd1 -85.0(3) . 2_756
O4 Pd2 N2 Pd1 -114.1(8) . 2_756
O5 Pd2 N2 Pd1 92.9(2) . 2_756
P1 Pd2 N2 Pd1 -93.0(3) . 2_756
Pd1 Pd2 N2 Pd1 50.2(3) . 2_756
Pd3 Pd2 N2 Pd1 -43.5(2) . 2_756
P1 N2 C21 C22 61.8(6) . .
Pd1 N2 C21 C22 174.1(4) 2_756 .
Pd2 N2 C21 C22 -50.6(6) . .
P1 N2 C21 C23 -64.2(6) . .
Pd1 N2 C21 C23 48.1(6) 2_756 .
Pd2 N2 C21 C23 -176.6(4) . .
O11 P1 N3 C31 7.6(7) . .
N1 P1 N3 C31 -123.1(6) . .
N2 P1 N3 C31 139.6(6) . .
Pd2 P1 N3 C31 130.0(6) . .
Pd1 P1 N3 C31 -170.9(5) 2_756 .
Pd3 P1 N3 C31 -130.0(6) . .
O11 P1 N3 Pd2 -122.4(3) . .
N1 P1 N3 Pd2 106.9(2) . .
N2 P1 N3 Pd2 9.7(2) . .
Pd1 P1 N3 Pd2 59.1(2) 2_756 .
Pd3 P1 N3 Pd2 100.0(2) . .
O11 P1 N3 Pd3 137.6(3) . .
N1 P1 N3 Pd3 7.0(2) . .
N2 P1 N3 Pd3 -90.3(2) . .
Pd2 P1 N3 Pd3 -100.0(2) . .
Pd1 P1 N3 Pd3 -40.8(2) 2_756 .
O4 Pd2 N3 C31 30.7(5) . .
O5 Pd2 N3 C31 -163.7(17) . .
N2 Pd2 N3 C31 -142.7(5) . .
P1 Pd2 N3 C31 -134.5(6) . .
Pd1 Pd2 N3 C31 107.2(4) . .
Pd3 Pd2 N3 C31 131.2(5) . .
O4 Pd2 N3 P1 165.3(2) . .
O5 Pd2 N3 P1 -29(2) . .
N2 Pd2 N3 P1 -8.1(2) . .
Pd1 Pd2 N3 P1 -118.24(19) . .
Pd3 Pd2 N3 P1 -94.3(2) . .
O4 Pd2 N3 Pd3 -100.5(2) . .
O5 Pd2 N3 Pd3 65(2) . .
N2 Pd2 N3 Pd3 86.1(2) . .
P1 Pd2 N3 Pd3 94.3(2) . .
Pd1 Pd2 N3 Pd3 -24.0(3) . .
O2 Pd3 N3 C31 -44.5(4) 2_756 .
O1 Pd3 N3 C31 101.8(13) . .
N1 Pd3 N3 C31 128.7(4) . .
P1 Pd3 N3 C31 134.5(5) . .
Pd1 Pd3 N3 C31 168.7(4) 2_756 .
Pd2 Pd3 N3 C31 -131.1(5) . .
O2 Pd3 N3 P1 -179.0(2) 2_756 .
O1 Pd3 N3 P1 -32.7(14) . .
N1 Pd3 N3 P1 -5.9(2) . .
Pd1 Pd3 N3 P1 34.16(18) 2_756 .
Pd2 Pd3 N3 P1 94.3(3) . .
O2 Pd3 N3 Pd2 86.7(2) 2_756 .
O1 Pd3 N3 Pd2 -127.0(12) . .
N1 Pd3 N3 Pd2 -100.2(2) . .
P1 Pd3 N3 Pd2 -94.3(3) . .
Pd1 Pd3 N3 Pd2 -60.16(16) 2_756 .
P1 N3 C31 C32 -64.3(7) . .
Pd2 N3 C31 C32 54.8(6) . .
Pd3 N3 C31 C32 176.7(4) . .
P1 N3 C31 C33 61.2(8) . .
Pd2 N3 C31 C33 -179.7(5) . .
Pd3 N3 C31 C33 -57.8(6) . .
