#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:26:18 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178899 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/28/4112890.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_4112890
loop_
_publ_author_name
'Biswaroop Chatterjee'
'Juan C. Noveron'
'Marino J. E. Resendiz'
'Jie Liu'
'Takuya Yamamoto'
'Daniel Parker'
'Martin Cinke'
'Cattien V. Nguyen'
'Atta M. Arif'
'Peter J. Stang'
_publ_section_title
;
 Self-Assembly of Flexible Supramolecular Metallacyclic Ensembles:
 Structures and Adsorption Properties of Their Nanoporous Crystalline
 Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10645
_journal_page_last               10656
_journal_paper_doi               10.1021/ja0388919
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C90 H92 F12 N4 O24 P4 Pd2 S4'
_chemical_formula_weight         2306.60
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.9466(10)
_cell_angle_beta                 104.8438(12)
_cell_angle_gamma                90.2628(20)
_cell_formula_units_Z            1
_cell_length_a                   10.5043(2)
_cell_length_b                   12.0394(3)
_cell_length_c                   20.2334(6)
_cell_measurement_reflns_used    2853
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     2471.77(11)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi plus Omega scan'
_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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.1041
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12126
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.04
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.8384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         9915
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0551
_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)+(0.0351P)²+4.2099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                7152
_reflns_number_total             9915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0388919si20040709_024047_3.cif
_cod_data_source_block           complex6
_cod_database_code               4112890
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Pd1 Pd 0.10998(3) 0.17408(3) 0.247682(18) 0.01897(11) Uani 1 1 d .
S1 S 0.55416(11) 0.39454(10) 0.36534(6) 0.0273(3) Uani 1 1 d .
S2 S 0.83793(16) 0.99515(12) 0.08807(9) 0.0510(4) Uani 1 1 d .
P1 P 0.02325(11) 0.08457(9) 0.32337(6) 0.0205(3) Uani 1 1 d .
P2 P -0.03680(11) 0.31158(9) 0.24637(6) 0.0197(3) Uani 1 1 d .
F1 F 0.6066(3) 0.6071(3) 0.3718(2) 0.0580(10) Uani 1 1 d .
F2 F 0.4896(4) 0.5594(3) 0.43874(19) 0.0587(10) Uani 1 1 d .
F3 F 0.4021(3) 0.5645(3) 0.3310(2) 0.0591(10) Uani 1 1 d .
F4 F 0.6003(5) 0.9321(4) 0.0349(4) 0.161(3) Uani 1 1 d .
F5 F 0.6595(5) 0.9677(4) 0.1472(3) 0.1004(16) Uani 1 1 d .
F6 F 0.6232(5) 1.1023(4) 0.0735(4) 0.148(3) Uani 1 1 d .
O1 O 0.5312(3) 0.3693(3) 0.05544(19) 0.0413(9) Uani 1 1 d .
O2 O 0.3537(3) 0.3191(3) -0.02897(16) 0.0297(8) Uani 1 1 d .
O3 O 0.4867(3) 0.2770(2) -0.20910(17) 0.0283(8) Uani 1 1 d .
O4 O 0.3326(3) 0.1692(3) -0.28132(18) 0.0352(8) Uani 1 1 d .
O5 O 0.6667(3) 0.3763(3) 0.42111(19) 0.0427(9) Uani 1 1 d .
O6 O 0.5795(3) 0.3965(3) 0.29822(17) 0.0324(8) Uani 1 1 d .
O7 O 0.4384(3) 0.3317(3) 0.36831(19) 0.0343(8) Uani 1 1 d .
O8 O 0.8343(7) 1.0330(5) 0.0135(3) 0.110(2) Uani 1 1 d .
O9 O 0.8777(4) 0.8829(3) 0.0974(2) 0.0485(10) Uani 1 1 d .
O10 O 0.9024(4) 1.0749(3) 0.1385(2) 0.0469(10) Uani 1 1 d .
O11 O 0.6792(6) 0.1328(4) 0.4352(4) 0.0941(19) Uani 1 1 d .
H11 H 0.6862 0.2024 0.4385 0.141 Uiso 1 1 calc R
O12 O 0.8931(5) 1.2082(4) -0.0619(3) 0.0780(15) Uani 1 1 d D
H12A H 0.976(6) 1.159(6) -0.074(4) 0.117 Uiso 1 1 d D
H12B H 0.867(8) 1.139(5) -0.030(4) 0.117 Uiso 1 1 d D
N1 N 0.1949(3) 0.2469(3) 0.17533(19) 0.0202(8) Uani 1 1 d .
N2 N 0.7451(3) -0.0510(3) -0.24858(19) 0.0205(8) Uani 1 1 d .
C1 C 0.3106(5) 0.3011(4) 0.1970(2) 0.0275(11) Uani 1 1 d .
H1 H 0.3430 0.3195 0.2444 0.033 Uiso 1 1 calc R
C2 C 0.3842(5) 0.3313(4) 0.1527(2) 0.0273(11) Uani 1 1 d .
H2 H 0.4657 0.3699 0.1695 0.033 Uiso 1 1 calc R
C3 C 0.3378(4) 0.3045(3) 0.0836(2) 0.0234(10) Uani 1 1 d .
C4 C 0.2162(4) 0.2499(4) 0.0609(2) 0.0248(10) Uani 1 1 d .
H4 H 0.1805 0.2321 0.0137 0.030 Uiso 1 1 calc R
C5 C 0.1489(4) 0.2224(4) 0.1084(2) 0.0248(10) Uani 1 1 d .
H5 H 0.0665 0.1845 0.0929 0.030 Uiso 1 1 calc R
C6 C 0.4197(5) 0.3346(4) 0.0359(3) 0.0282(11) Uani 1 1 d .
C7 C 0.4243(5) 0.3438(4) -0.0798(3) 0.0333(12) Uani 1 1 d .
H7A H 0.4950 0.2892 -0.0787 0.040 Uiso 1 1 calc R
H7B H 0.4646 0.4191 -0.0709 0.040 Uiso 1 1 calc R
C8 C 0.3249(5) 0.3372(4) -0.1480(2) 0.0296(11) Uani 1 1 d .
H8A H 0.2549 0.3920 -0.1480 0.035 Uiso 1 1 calc R
H8B H 0.2835 0.2622 -0.1553 0.035 Uiso 1 1 calc R
C9 C 0.3863(5) 0.3597(4) -0.2060(3) 0.0331(12) Uani 1 1 d .
H9A H 0.3173 0.3572 -0.2498 0.040 Uiso 1 1 calc R
H9B H 0.4271 0.4349 -0.1993 0.040 Uiso 1 1 calc R
C10 C 0.4428(5) 0.1860(4) -0.2487(3) 0.0271(11) Uani 1 1 d .
C11 C 0.5527(4) 0.1045(4) -0.2468(2) 0.0233(10) Uani 1 1 d .
C12 C 0.5240(5) 0.0101(4) -0.2897(3) 0.0276(11) Uani 1 1 d .
H12 H 0.4385 -0.0018 -0.3193 0.033 Uiso 1 1 calc R
C13 C 0.6225(4) -0.0660(4) -0.2885(3) 0.0273(11) Uani 1 1 d .
H13 H 0.6026 -0.1314 -0.3170 0.033 Uiso 1 1 calc R
C14 C 0.7727(4) 0.0397(4) -0.2066(2) 0.0247(10) Uani 1 1 d .
H14 H 0.8590 0.0494 -0.1775 0.030 Uiso 1 1 calc R
C15 C 0.6789(4) 0.1194(4) -0.2046(2) 0.0270(11) Uani 1 1 d .
H15 H 0.7006 0.1832 -0.1749 0.032 Uiso 1 1 calc R
C16 C -0.1553(4) 0.0838(4) 0.3042(3) 0.0250(10) Uani 1 1 d .
H16A H -0.1906 0.0427 0.2600 0.030 Uiso 1 1 calc R
H16B H -0.1825 0.0424 0.3399 0.030 Uiso 1 1 calc R
C17 C -0.2184(4) 0.1982(4) 0.3000(3) 0.0268(11) Uani 1 1 d .
H17A H -0.3133 0.1888 0.2973 0.032 Uiso 1 1 calc R
H17B H -0.1779 0.2420 0.3425 0.032 Uiso 1 1 calc R
C18 C -0.2041(4) 0.2633(4) 0.2389(2) 0.0228(10) Uani 1 1 d .
H18A H -0.2628 0.3283 0.2340 0.027 Uiso 1 1 calc R
H18B H -0.2333 0.2155 0.1968 0.027 Uiso 1 1 calc R
C19 C 0.0864(5) 0.1340(3) 0.4113(2) 0.0250(10) Uani 1 1 d .
C20 C 0.2160(5) 0.1729(4) 0.4335(3) 0.0295(11) Uani 1 1 d .
H20 H 0.2681 0.1777 0.4015 0.035 Uiso 1 1 calc R
C21 C 0.2700(5) 0.2047(4) 0.5010(3) 0.0389(13) Uani 1 1 d .
H21 H 0.3585 0.2312 0.5156 0.047 Uiso 1 1 calc R
C22 C 0.1943(6) 0.1977(4) 0.5474(3) 0.0392(13) Uani 1 1 d .
H22 H 0.2318 0.2176 0.5942 0.047 Uiso 1 1 calc R
C23 C 0.0645(6) 0.1619(4) 0.5263(3) 0.0440(14) Uani 1 1 d .
H23 H 0.0123 0.1592 0.5582 0.053 Uiso 1 1 calc R
C24 C 0.0110(6) 0.1300(4) 0.4586(3) 0.0368(13) Uani 1 1 d .
H24 H -0.0781 0.1051 0.4442 0.044 Uiso 1 1 calc R
C25 C 0.0642(4) -0.0618(4) 0.3222(2) 0.0241(10) Uani 1 1 d .
C26 C -0.0120(5) -0.1342(4) 0.2731(3) 0.0320(12) Uani 1 1 d .
H26 H -0.0883 -0.1080 0.2416 0.038 Uiso 1 1 calc R
C27 C 0.0228(5) -0.2451(4) 0.2697(3) 0.0388(13) Uani 1 1 d .
H27 H -0.0300 -0.2944 0.2359 0.047 Uiso 1 1 calc R
C28 C 0.1329(5) -0.2837(4) 0.3149(3) 0.0393(13) Uani 1 1 d .
H28 H 0.1561 -0.3596 0.3126 0.047 Uiso 1 1 calc R
C29 C 0.2092(6) -0.2123(4) 0.3633(3) 0.0438(14) Uani 1 1 d .
H29 H 0.2860 -0.2388 0.3943 0.053 Uiso 1 1 calc R
C30 C 0.1749(5) -0.1012(4) 0.3675(3) 0.0353(12) Uani 1 1 d .
H30 H 0.2278 -0.0524 0.4016 0.042 Uiso 1 1 calc R
C31 C 0.0070(4) 0.4034(3) 0.3218(2) 0.0213(10) Uani 1 1 d .
C32 C 0.1359(5) 0.4093(4) 0.3617(3) 0.0286(11) Uani 1 1 d .
H32 H 0.2015 0.3653 0.3492 0.034 Uiso 1 1 calc R
C33 C 0.1700(5) 0.4791(4) 0.4199(3) 0.0307(11) Uani 1 1 d .
H33 H 0.2585 0.4826 0.4470 0.037 Uiso 1 1 calc R
C34 C 0.0759(5) 0.5428(4) 0.4383(3) 0.0319(11) Uani 1 1 d .
H34 H 0.0993 0.5907 0.4779 0.038 Uiso 1 1 calc R
C35 C -0.0522(5) 0.5376(4) 0.3994(3) 0.0329(12) Uani 1 1 d .
H35 H -0.1168 0.5822 0.4124 0.039 Uiso 1 1 calc R
C36 C -0.0883(5) 0.4681(4) 0.3415(3) 0.0277(11) Uani 1 1 d .
H36 H -0.1774 0.4642 0.3154 0.033 Uiso 1 1 calc R
C37 C -0.0490(4) 0.3990(4) 0.1743(2) 0.0251(10) Uani 1 1 d .
C38 C -0.1431(5) 0.3806(4) 0.1127(3) 0.0343(12) Uani 1 1 d .
H38 H -0.2043 0.3206 0.1077 0.041 Uiso 1 1 calc R
C39 C -0.1485(6) 0.4491(5) 0.0585(3) 0.0454(15) Uani 1 1 d .
H39 H -0.2134 0.4362 0.0166 0.055 Uiso 1 1 calc R
C40 C -0.0593(6) 0.5362(5) 0.0653(3) 0.0445(15) Uani 1 1 d .
H40 H -0.0638 0.5838 0.0283 0.053 Uiso 1 1 calc R
C41 C 0.0353(6) 0.5539(4) 0.1254(3) 0.0461(15) Uani 1 1 d .
H41 H 0.0966 0.6136 0.1293 0.055 Uiso 1 1 calc R
C42 C 0.0435(5) 0.4872(4) 0.1801(3) 0.0358(12) Uani 1 1 d .
H42 H 0.1104 0.5001 0.2213 0.043 Uiso 1 1 calc R
C43 C 0.5109(5) 0.5384(4) 0.3775(3) 0.0355(12) Uani 1 1 d .
C44 C 0.6722(8) 0.9969(6) 0.0878(5) 0.078(2) Uani 1 1 d .
C45 C 0.5836(8) 0.0988(7) 0.4648(4) 0.085(3) Uani 1 1 d .
H45A H 0.6099 0.1184 0.5139 0.127 Uiso 1 1 calc R
H45B H 0.5714 0.0181 0.4583 0.127 Uiso 1 1 calc R
H45C H 0.5008 0.1355 0.4437 0.127 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'
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'
F F 0.0171 0.0103 '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 N2 83.31(14) . 2_655
N1 Pd1 P2 94.49(10) . .
N2 Pd1 P2 177.18(10) 2_655 .
N1 Pd1 P1 176.17(10) . .
N2 Pd1 P1 93.26(10) 2_655 .
P2 Pd1 P1 88.99(4) . .
O5 S1 O7 113.9(2) . .
O5 S1 O6 115.6(2) . .
O7 S1 O6 115.0(2) . .
O5 S1 C43 104.6(2) . .
O7 S1 C43 104.3(2) . .
O6 S1 C43 101.2(2) . .
O10 S2 O9 117.3(3) . .
O10 S2 O8 111.6(3) . .
O9 S2 O8 111.6(3) . .
O10 S2 C44 106.6(3) . .
O9 S2 C44 106.0(3) . .
O8 S2 C44 102.2(4) . .
C19 P1 C16 107.8(2) . .
C19 P1 C25 105.6(2) . .
C16 P1 C25 103.8(2) . .
C19 P1 Pd1 114.02(15) . .
C16 P1 Pd1 115.08(16) . .
C25 P1 Pd1 109.58(15) . .
C37 P2 C31 106.0(2) . .
C37 P2 C18 104.9(2) . .
C31 P2 C18 106.4(2) . .
C37 P2 Pd1 111.43(15) . .
C31 P2 Pd1 113.03(14) . .
C18 P2 Pd1 114.39(14) . .
C6 O2 C7 116.4(4) . .
C10 O3 C9 115.2(4) . .
C45 O11 H11 109.5 . .
H12A O12 H12B 92(6) . .
C5 N1 C1 118.6(4) . .
C5 N1 Pd1 120.9(3) . .
C1 N1 Pd1 119.3(3) . .
C13 N2 C14 119.1(4) . .
C13 N2 Pd1 120.2(3) . 2_655
C14 N2 Pd1 120.7(3) . 2_655
N1 C1 C2 122.2(4) . .
N1 C1 H1 118.9 . .
C2 C1 H1 118.9 . .
C1 C2 C3 119.2(4) . .
C1 C2 H2 120.4 . .
C3 C2 H2 120.4 . .
C2 C3 C4 118.5(4) . .
C2 C3 C6 119.2(4) . .
C4 C3 C6 122.4(4) . .
C5 C4 C3 118.8(4) . .
C5 C4 H4 120.6 . .
C3 C4 H4 120.6 . .
N1 C5 C4 122.6(4) . .
N1 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
O1 C6 O2 125.3(5) . .
O1 C6 C3 123.0(5) . .
O2 C6 C3 111.7(4) . .
O2 C7 C8 106.6(4) . .
O2 C7 H7A 110.4 . .
C8 C7 H7A 110.4 . .
O2 C7 H7B 110.4 . .
C8 C7 H7B 110.4 . .
H7A C7 H7B 108.6 . .
C7 C8 C9 112.0(4) . .
C7 C8 H8A 109.2 . .
C9 C8 H8A 109.2 . .
C7 C8 H8B 109.2 . .
C9 C8 H8B 109.2 . .
H8A C8 H8B 107.9 . .
O3 C9 C8 110.5(4) . .
O3 C9 H9A 109.6 . .
C8 C9 H9A 109.6 . .
O3 C9 H9B 109.6 . .
C8 C9 H9B 109.6 . .
H9A C9 H9B 108.1 . .
O4 C10 O3 125.7(4) . .
O4 C10 C11 123.1(4) . .
O3 C10 C11 111.2(4) . .
C15 C11 C12 119.1(4) . .
C15 C11 C10 123.4(4) . .
C12 C11 C10 117.5(4) . .
C13 C12 C11 118.6(4) . .
C13 C12 H12 120.7 . .
C11 C12 H12 120.7 . .
N2 C13 C12 122.4(4) . .
N2 C13 H13 118.8 . .
C12 C13 H13 118.8 . .
N2 C14 C15 121.9(4) . .
N2 C14 H14 119.1 . .
C15 C14 H14 119.1 . .
C14 C15 C11 119.0(4) . .
C14 C15 H15 120.5 . .
C11 C15 H15 120.5 . .
C17 C16 P1 115.4(3) . .
C17 C16 H16A 108.4 . .
P1 C16 H16A 108.4 . .
C17 C16 H16B 108.4 . .
P1 C16 H16B 108.4 . .
H16A C16 H16B 107.5 . .
C18 C17 C16 113.9(4) . .
C18 C17 H17A 108.8 . .
C16 C17 H17A 108.8 . .
C18 C17 H17B 108.8 . .
C16 C17 H17B 108.8 . .
H17A C17 H17B 107.7 . .
C17 C18 P2 113.3(3) . .
C17 C18 H18A 108.9 . .
P2 C18 H18A 108.9 . .
C17 C18 H18B 108.9 . .
P2 C18 H18B 108.9 . .
H18A C18 H18B 107.7 . .
C24 C19 C20 118.5(5) . .
C24 C19 P1 122.0(4) . .
C20 C19 P1 119.5(4) . .
C21 C20 C19 121.1(5) . .
C21 C20 H20 119.5 . .
C19 C20 H20 119.5 . .
C20 C21 C22 119.4(5) . .
C20 C21 H21 120.3 . .
C22 C21 H21 120.3 . .
C21 C22 C23 120.6(5) . .
C21 C22 H22 119.7 . .
C23 C22 H22 119.7 . .
C24 C23 C22 119.8(5) . .
C24 C23 H23 120.1 . .
C22 C23 H23 120.1 . .
C23 C24 C19 120.6(5) . .
C23 C24 H24 119.7 . .
C19 C24 H24 119.7 . .
C30 C25 C26 119.1(4) . .
C30 C25 P1 120.8(4) . .
C26 C25 P1 119.9(4) . .
C25 C26 C27 120.2(5) . .
C25 C26 H26 119.9 . .
C27 C26 H26 119.9 . .
C28 C27 C26 120.3(5) . .
C28 C27 H27 119.8 . .
C26 C27 H27 119.8 . .
C29 C28 C27 119.7(5) . .
C29 C28 H28 120.2 . .
C27 C28 H28 120.2 . .
C28 C29 C30 120.5(5) . .
C28 C29 H29 119.8 . .
C30 C29 H29 119.8 . .
C25 C30 C29 120.1(5) . .
C25 C30 H30 119.9 . .
C29 C30 H30 119.9 . .
C32 C31 C36 118.9(4) . .
C32 C31 P2 120.3(3) . .
C36 C31 P2 120.9(3) . .
C31 C32 C33 120.5(4) . .
C31 C32 H32 119.7 . .
C33 C32 H32 119.7 . .
C34 C33 C32 120.0(5) . .
C34 C33 H33 120.0 . .
C32 C33 H33 120.0 . .
C33 C34 C35 120.1(5) . .
C33 C34 H34 119.9 . .
C35 C34 H34 119.9 . .
C34 C35 C36 120.8(5) . .
C34 C35 H35 119.6 . .
C36 C35 H35 119.6 . .
C35 C36 C31 119.7(4) . .
C35 C36 H36 120.2 . .
C31 C36 H36 120.1 . .
C38 C37 C42 118.9(5) . .
C38 C37 P2 122.3(4) . .
C42 C37 P2 118.8(4) . .
C39 C38 C37 120.4(5) . .
C39 C38 H38 119.8 . .
C37 C38 H38 119.8 . .
C40 C39 C38 120.1(6) . .
C40 C39 H39 120.0 . .
C38 C39 H39 120.0 . .
C41 C40 C39 120.0(5) . .
C41 C40 H40 120.0 . .
C39 C40 H40 120.0 . .
C40 C41 C42 121.4(6) . .
C40 C41 H41 119.3 . .
C42 C41 H41 119.3 . .
C41 C42 C37 119.2(5) . .
C41 C42 H42 120.4 . .
C37 C42 H42 120.4 . .
F3 C43 F1 107.9(5) . .
F3 C43 F2 107.3(4) . .
F1 C43 F2 107.0(4) . .
F3 C43 S1 110.8(4) . .
F1 C43 S1 111.0(4) . .
F2 C43 S1 112.6(4) . .
F5 C44 F4 113.2(7) . .
F5 C44 F6 110.5(8) . .
F4 C44 F6 103.8(7) . .
F5 C44 S2 109.3(6) . .
F4 C44 S2 110.3(6) . .
F6 C44 S2 109.5(6) . .
O11 C45 H45A 109.5 . .
O11 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
O11 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 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 2.111(4) .
Pd1 N2 2.126(3) 2_655
Pd1 P2 2.2635(11) .
Pd1 P1 2.2705(12) .
S1 O5 1.434(4) .
S1 O7 1.445(3) .
S1 O6 1.450(3) .
S1 C43 1.817(5) .
S2 O10 1.413(4) .
S2 O9 1.420(4) .
S2 O8 1.581(6) .
S2 C44 1.740(9) .
P1 C19 1.810(5) .
P1 C16 1.815(4) .
P1 C25 1.816(4) .
P2 C37 1.806(5) .
P2 C31 1.813(4) .
P2 C18 1.816(4) .
F1 C43 1.329(6) .
F2 C43 1.331(6) .
F3 C43 1.327(6) .
F4 C44 1.359(9) .
F5 C44 1.302(9) .
F6 C44 1.383(9) .
O1 C6 1.205(5) .
O2 C6 1.323(6) .
O2 C7 1.452(5) .
O3 C10 1.342(6) .
O3 C9 1.465(5) .
O4 C10 1.190(6) .
O11 C45 1.363(8) .
O11 H11 0.8400 .
O12 H12A 1.13(2) .
O12 H12B 1.15(2) .
N1 C5 1.339(6) .
N1 C1 1.340(5) .
N2 C13 1.342(6) .
N2 C14 1.342(5) .
N2 Pd1 2.126(3) 2_655
C1 C2 1.380(6) .
C1 H1 0.9500 .
C2 C3 1.385(6) .
C2 H2 0.9500 .
C3 C4 1.394(6) .
C3 C6 1.500(7) .
C4 C5 1.378(6) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C7 C8 1.502(7) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.508(7) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.512(6) .
C11 C15 1.387(6) .
C11 C12 1.390(6) .
C12 C13 1.381(6) .
C12 H12 0.9500 .
C13 H13 0.9500 .
C14 C15 1.386(6) .
C14 H14 0.9500 .
C15 H15 0.9500 .
C16 C17 1.526(6) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.525(6) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C24 1.393(7) .
C19 C20 1.394(6) .
C20 C21 1.379(7) .
C20 H20 0.9500 .
C21 C22 1.380(7) .
C21 H21 0.9500 .
C22 C23 1.383(8) .
C22 H22 0.9500 .
C23 C24 1.380(7) .
C23 H23 0.9500 .
C24 H24 0.9500 .
C25 C30 1.380(7) .
C25 C26 1.384(6) .
C26 C27 1.390(6) .
C26 H26 0.9500 .
C27 C28 1.371(7) .
C27 H27 0.9500 .
C28 C29 1.370(7) .
C28 H28 0.9500 .
C29 C30 1.393(7) .
C29 H29 0.9500 .
C30 H30 0.9500 .
C31 C32 1.388(6) .
C31 C36 1.400(6) .
C32 C33 1.391(6) .
C32 H32 0.9500 .
C33 C34 1.371(7) .
C33 H33 0.9500 .
C34 C35 1.373(7) .
C34 H34 0.9500 .
C35 C36 1.385(6) .
C35 H35 0.9500 .
C36 H36 0.9500 .
C37 C38 1.389(7) .
C37 C42 1.418(7) .
C38 C39 1.384(7) .
C38 H38 0.9500 .
C39 C40 1.382(8) .
C39 H39 0.9500 .
C40 C41 1.368(8) .
C40 H40 0.9500 .
C41 C42 1.375(7) .
C41 H41 0.9500 .
C42 H42 0.9500 .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 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
O11 H11 O5 0.84 2.14 2.956(6) 164.7 .
O12 H12B O8 1.15(2) 1.66(2) 2.802(8) 176(7) .
O12 H12A O9 1.13(2) 1.79(3) 2.894(7) 164(7) 2_775
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
N1 Pd1 P1 C19 122.2(16) .
N2 Pd1 P1 C19 95.86(19) 2_655
P2 Pd1 P1 C19 -82.44(16) .
N1 Pd1 P1 C16 -112.5(16) .
N2 Pd1 P1 C16 -138.82(19) 2_655
P2 Pd1 P1 C16 42.88(17) .
N1 Pd1 P1 C25 4.1(16) .
N2 Pd1 P1 C25 -22.27(19) 2_655
P2 Pd1 P1 C25 159.43(17) .
N1 Pd1 P2 C37 14.2(2) .
N2 Pd1 P2 C37 53(2) 2_655
P1 Pd1 P2 C37 -164.21(17) .
N1 Pd1 P2 C31 -105.03(18) .
N2 Pd1 P2 C31 -66(2) 2_655
P1 Pd1 P2 C31 76.57(16) .
N1 Pd1 P2 C18 132.9(2) .
N2 Pd1 P2 C18 172(2) 2_655
P1 Pd1 P2 C18 -45.47(18) .
N2 Pd1 N1 C5 90.7(3) 2_655
P2 Pd1 N1 C5 -91.0(3) .
P1 Pd1 N1 C5 64.2(17) .
N2 Pd1 N1 C1 -76.5(3) 2_655
P2 Pd1 N1 C1 101.7(3) .
P1 Pd1 N1 C1 -103.0(15) .
C5 N1 C1 C2 -0.7(7) .
Pd1 N1 C1 C2 166.8(3) .
N1 C1 C2 C3 -0.2(7) .
C1 C2 C3 C4 1.4(7) .
C1 C2 C3 C6 -178.4(4) .
C2 C3 C4 C5 -1.6(6) .
C6 C3 C4 C5 178.1(4) .
C1 N1 C5 C4 0.5(7) .
Pd1 N1 C5 C4 -166.8(3) .
C3 C4 C5 N1 0.7(7) .
C7 O2 C6 O1 1.6(7) .
C7 O2 C6 C3 -179.0(4) .
C2 C3 C6 O1 9.1(7) .
C4 C3 C6 O1 -170.7(5) .
C2 C3 C6 O2 -170.3(4) .
C4 C3 C6 O2 9.9(6) .
C6 O2 C7 C8 -171.5(4) .
O2 C7 C8 C9 -179.2(4) .
C10 O3 C9 C8 90.1(5) .
C7 C8 C9 O3 61.2(5) .
C9 O3 C10 O4 1.5(7) .
C9 O3 C10 C11 -178.3(4) .
O4 C10 C11 C15 -174.6(5) .
O3 C10 C11 C15 5.1(6) .
O4 C10 C11 C12 5.3(7) .
O3 C10 C11 C12 -174.9(4) .
C15 C11 C12 C13 0.4(7) .
C10 C11 C12 C13 -179.5(4) .
C14 N2 C13 C12 2.0(7) .
Pd1 N2 C13 C12 178.4(4) 2_655
C11 C12 C13 N2 -1.5(7) .
C13 N2 C14 C15 -1.5(7) .
Pd1 N2 C14 C15 -177.9(3) 2_655
N2 C14 C15 C11 0.6(7) .
C12 C11 C15 C14 0.0(7) .
C10 C11 C15 C14 179.9(4) .
C19 P1 C16 C17 69.8(4) .
C25 P1 C16 C17 -178.5(4) .
Pd1 P1 C16 C17 -58.7(4) .
P1 C16 C17 C18 68.1(5) .
C16 C17 C18 P2 -70.6(4) .
C37 P2 C18 C17 -173.3(3) .
C31 P2 C18 C17 -61.3(3) .
Pd1 P2 C18 C17 64.3(3) .
C16 P1 C19 C24 21.2(4) .
C25 P1 C19 C24 -89.4(4) .
Pd1 P1 C19 C24 150.3(3) .
C16 P1 C19 C20 -161.6(4) .
C25 P1 C19 C20 87.8(4) .
Pd1 P1 C19 C20 -32.6(4) .
C24 C19 C20 C21 1.4(7) .
P1 C19 C20 C21 -175.9(4) .
C19 C20 C21 C22 0.0(8) .
C20 C21 C22 C23 -1.6(8) .
C21 C22 C23 C24 1.8(8) .
C22 C23 C24 C19 -0.3(8) .
C20 C19 C24 C23 -1.3(7) .
P1 C19 C24 C23 175.9(4) .
C19 P1 C25 C30 -30.1(5) .
C16 P1 C25 C30 -143.5(4) .
Pd1 P1 C25 C30 93.1(4) .
C19 P1 C25 C26 153.4(4) .
C16 P1 C25 C26 40.0(4) .
Pd1 P1 C25 C26 -83.4(4) .
C30 C25 C26 C27 0.1(8) .
P1 C25 C26 C27 176.7(4) .
C25 C26 C27 C28 -0.1(8) .
C26 C27 C28 C29 -0.3(9) .
C27 C28 C29 C30 0.7(9) .
C26 C25 C30 C29 0.3(8) .
P1 C25 C30 C29 -176.2(4) .
C28 C29 C30 C25 -0.7(9) .
C37 P2 C31 C32 -101.9(4) .
C18 P2 C31 C32 146.9(4) .
Pd1 P2 C31 C32 20.5(4) .
C37 P2 C31 C36 79.2(4) .
C18 P2 C31 C36 -32.1(4) .
Pd1 P2 C31 C36 -158.5(3) .
C36 C31 C32 C33 -0.6(7) .
P2 C31 C32 C33 -179.6(4) .
C31 C32 C33 C34 0.0(7) .
C32 C33 C34 C35 0.2(8) .
C33 C34 C35 C36 0.2(8) .
C34 C35 C36 C31 -0.9(7) .
C32 C31 C36 C35 1.1(7) .
P2 C31 C36 C35 -180.0(4) .
C31 P2 C37 C38 -143.1(4) .
C18 P2 C37 C38 -30.7(4) .
Pd1 P2 C37 C38 93.6(4) .
C31 P2 C37 C42 39.1(4) .
C18 P2 C37 C42 151.4(4) .
Pd1 P2 C37 C42 -84.3(4) .
C42 C37 C38 C39 -1.6(7) .
P2 C37 C38 C39 -179.5(4) .
C37 C38 C39 C40 0.3(8) .
C38 C39 C40 C41 0.8(8) .
C39 C40 C41 C42 -0.7(8) .
C40 C41 C42 C37 -0.7(8) .
C38 C37 C42 C41 1.8(7) .
P2 C37 C42 C41 179.7(4) .
O5 S1 C43 F3 -176.2(3) .
O7 S1 C43 F3 -56.3(4) .
O6 S1 C43 F3 63.3(4) .
O5 S1 C43 F1 63.9(4) .
O7 S1 C43 F1 -176.2(4) .
O6 S1 C43 F1 -56.6(4) .
O5 S1 C43 F2 -56.1(4) .
O7 S1 C43 F2 63.8(4) .
O6 S1 C43 F2 -176.6(4) .
O10 S2 C44 F5 -62.3(6) .
O9 S2 C44 F5 63.4(6) .
O8 S2 C44 F5 -179.6(5) .
O10 S2 C44 F4 172.6(6) .
O9 S2 C44 F4 -61.7(7) .
O8 S2 C44 F4 55.3(7) .
O10 S2 C44 F6 58.9(7) .
O9 S2 C44 F6 -175.3(5) .
O8 S2 C44 F6 -58.3(7) .
