#------------------------------------------------------------------------------
#$Date: 2017-07-11 14:26:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198632 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/17/4101785.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_4101785
loop_
_publ_author_name
'Ramesh Giri'
'Jonathan K. Lam'
'Jin-Quan Yu'
_publ_section_title
;
 Synthetic Applications of Pd(II)-Catalyzed C-H Carboxylation and
 Mechanistic Insights: Expedient Routes to Anthranilic Acids,
 Oxazolinones, and Quinazolinones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              686
_journal_page_last               693
_journal_paper_doi               10.1021/ja9077705
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C19 H22 N O5 Pd S'
_chemical_formula_weight         482.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 98.100(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   57.31(2)
_cell_length_b                   7.522(3)
_cell_length_c                   18.203(7)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.73
_cell_volume                     7769(5)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35679
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  0.8276
_exptl_absorpt_correction_T_min  0.7212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.392
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         10746
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0385
_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)+(0.0534P)²+28.1147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                10308
_reflns_number_total             10746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9077705_si_001.cif
_cod_data_source_block           yu13a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        7768(5)
_cod_database_code               4101785
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'
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
C1 C 0.39540(13) 0.0608(9) 0.5361(4) 0.0246(16) Uani 1 1 d . . .
C2 C 0.40278(15) 0.1252(9) 0.4702(4) 0.0301(17) Uani 1 1 d . . .
C3 C 0.38666(13) 0.1876(9) 0.4117(4) 0.0277(17) Uani 1 1 d . . .
C4 C 0.36277(14) 0.1926(10) 0.4171(4) 0.0292(17) Uani 1 1 d . . .
C5 C 0.35477(12) 0.1296(9) 0.4807(4) 0.0278(16) Uani 1 1 d . . .
C6 C 0.37107(14) 0.0654(9) 0.5396(4) 0.0241(16) Uani 1 1 d . . .
C7 C 0.37183(14) -0.0908(8) 0.6584(4) 0.0253(16) Uani 1 1 d . . .
C8 C 0.35729(14) -0.1450(10) 0.7175(4) 0.0327(18) Uani 1 1 d . . .
H8A H 0.3617 -0.2653 0.7348 0.049 Uiso 1 1 calc R . .
H8B H 0.3405 -0.1429 0.6970 0.049 Uiso 1 1 calc R . .
H8C H 0.3601 -0.0619 0.7593 0.049 Uiso 1 1 calc R . .
C9 C 0.43949(13) -0.0908(10) 0.7826(4) 0.0330(16) Uani 1 1 d . . .
H9A H 0.4236 -0.1114 0.7962 0.040 Uiso 1 1 calc R . .
H9B H 0.4434 0.0371 0.7883 0.040 Uiso 1 1 calc R . .
C10 C 0.45784(14) -0.2055(10) 0.8284(4) 0.0367(18) Uani 1 1 d . . .
H10A H 0.4632 -0.1510 0.8774 0.044 Uiso 1 1 calc R . .
H10B H 0.4517 -0.3261 0.8358 0.044 Uiso 1 1 calc R . .
C11 C 0.47701(14) -0.2109(11) 0.7824(5) 0.042(2) Uani 1 1 d . . .
H11A H 0.4875 -0.3141 0.7957 0.050 Uiso 1 1 calc R . .
H11B H 0.4865 -0.1006 0.7884 0.050 Uiso 1 1 calc R . .
C12 C 0.46410(15) -0.2282(12) 0.7025(5) 0.038(2) Uani 1 1 d . . .
H12A H 0.4724 -0.1606 0.6672 0.045 Uiso 1 1 calc R . .
H12B H 0.4629 -0.3542 0.6868 0.045 Uiso 1 1 calc R . .
C13 C 0.48362(12) 0.2609(9) 0.5779(4) 0.0199(14) Uani 1 1 d . . .
C14 C 0.50352(11) 0.1948(8) 0.6213(4) 0.0212(14) Uani 1 1 d . . .
H14 H 0.5024 0.1419 0.6680 0.025 Uiso 1 1 calc R . .
C15 C 0.52529(12) 0.2072(9) 0.5950(4) 0.0281(16) Uani 1 1 d . . .
H15 H 0.5390 0.1608 0.6243 0.034 Uiso 1 1 calc R . .
C16 C 0.52725(12) 0.2843(9) 0.5285(4) 0.0235(15) Uani 1 1 d . . .
C17 C 0.50708(11) 0.3552(9) 0.4871(4) 0.0275(14) Uani 1 1 d . . .
H17 H 0.5083 0.4130 0.4414 0.033 Uiso 1 1 calc R . .
C18 C 0.48524(11) 0.3433(8) 0.5109(4) 0.0252(14) Uani 1 1 d . . .
H18 H 0.4716 0.3909 0.4818 0.030 Uiso 1 1 calc R . .
C19 C 0.55040(14) 0.3006(11) 0.5009(4) 0.0360(19) Uani 1 1 d . . .
H19A H 0.5629 0.2579 0.5390 0.054 Uiso 1 1 calc R . .
H19B H 0.5533 0.4255 0.4897 0.054 Uiso 1 1 calc R . .
H19C H 0.5502 0.2292 0.4558 0.054 Uiso 1 1 calc R . .
C20 C 0.36027(13) 0.4114(9) 0.6635(4) 0.0226(15) Uani 1 1 d . . .
C21 C 0.35294(12) 0.3526(9) 0.7294(4) 0.0240(16) Uani 1 1 d . . .
H21 H 0.3366 0.3561 0.7340 0.029 Uiso 1 1 calc R . .
C22 C 0.36865(14) 0.2895(10) 0.7881(4) 0.0329(18) Uani 1 1 d . . .
H22 H 0.3631 0.2478 0.8318 0.039 Uiso 1 1 calc R . .
C23 C 0.39251(14) 0.2873(10) 0.7828(5) 0.0333(18) Uani 1 1 d . . .
H23 H 0.4034 0.2432 0.8228 0.040 Uiso 1 1 calc R . .
C24 C 0.40043(13) 0.3495(9) 0.7190(4) 0.0301(17) Uani 1 1 d . . .
H24 H 0.4168 0.3480 0.7150 0.036 Uiso 1 1 calc R . .
C25 C 0.38446(14) 0.4134(10) 0.6615(4) 0.0264(17) Uani 1 1 d . . .
C26 C 0.38413(12) 0.5632(8) 0.5405(4) 0.0232(16) Uani 1 1 d . . .
C27 C 0.39837(13) 0.6177(10) 0.4833(4) 0.0273(16) Uani 1 1 d . . .
H27A H 0.3904 0.5821 0.4343 0.041 Uiso 1 1 calc R . .
H27B H 0.4138 0.5603 0.4926 0.041 Uiso 1 1 calc R . .
H27C H 0.4004 0.7471 0.4847 0.041 Uiso 1 1 calc R . .
C28 C 0.31607(15) 0.5967(13) 0.4188(5) 0.041(2) Uani 1 1 d . . .
H28A H 0.3123 0.4704 0.4076 0.050 Uiso 1 1 calc R . .
H28B H 0.3322 0.6213 0.4077 0.050 Uiso 1 1 calc R . .
C29 C 0.29845(17) 0.7166(14) 0.3744(6) 0.052(3) Uani 1 1 d . . .
H29A H 0.2930 0.6666 0.3247 0.063 Uiso 1 1 calc R . .
H29B H 0.3050 0.8369 0.3689 0.063 Uiso 1 1 calc R . .
C30 C 0.27848(15) 0.7196(13) 0.4234(5) 0.046(2) Uani 1 1 d . . .
H30A H 0.2695 0.8324 0.4169 0.055 Uiso 1 1 calc R . .
H30B H 0.2675 0.6191 0.4110 0.055 Uiso 1 1 calc R . .
C31 C 0.29083(16) 0.7030(11) 0.4998(5) 0.035(2) Uani 1 1 d . . .
H31A H 0.2918 0.8202 0.5249 0.043 Uiso 1 1 calc R . .
H31B H 0.2823 0.6198 0.5287 0.043 Uiso 1 1 calc R . .
C32 C 0.27190(11) 0.2131(9) 0.6214(4) 0.0188(14) Uani 1 1 d . . .
C33 C 0.25212(13) 0.2821(10) 0.5795(4) 0.0277(16) Uani 1 1 d . . .
H33 H 0.2533 0.3327 0.5324 0.033 Uiso 1 1 calc R . .
C34 C 0.23083(12) 0.2791(9) 0.6045(4) 0.0221(15) Uani 1 1 d . . .
H34 H 0.2174 0.3286 0.5750 0.027 Uiso 1 1 calc R . .
C35 C 0.22863(13) 0.2029(9) 0.6739(4) 0.0251(16) Uani 1 1 d . . .
C36 C 0.24841(13) 0.1321(10) 0.7153(4) 0.0285(16) Uani 1 1 d . . .
H36 H 0.2471 0.0798 0.7620 0.034 Uiso 1 1 calc R . .
C37 C 0.27007(13) 0.1347(10) 0.6910(4) 0.0264(16) Uani 1 1 d . . .
H37 H 0.2835 0.0850 0.7203 0.032 Uiso 1 1 calc R . .
C38 C 0.20517(14) 0.2040(11) 0.7020(5) 0.0343(19) Uani 1 1 d . . .
H38A H 0.2035 0.0950 0.7303 0.051 Uiso 1 1 calc R . .
H38B H 0.1925 0.2104 0.6599 0.051 Uiso 1 1 calc R . .
H38C H 0.2043 0.3075 0.7342 0.051 Uiso 1 1 calc R . .
C39 C 0.14446(13) 0.1121(10) 0.2880(4) 0.0275(16) Uani 1 1 d . . .
C40 C 0.15189(14) 0.1685(9) 0.2218(4) 0.0281(16) Uani 1 1 d . . .
H40 H 0.1681 0.1630 0.2167 0.034 Uiso 1 1 calc R . .
C41 C 0.13594(13) 0.2320(11) 0.1639(4) 0.0316(17) Uani 1 1 d . . .
H41 H 0.1413 0.2663 0.1189 0.038 Uiso 1 1 calc R . .
C42 C 0.11216(13) 0.2466(11) 0.1705(4) 0.0326(18) Uani 1 1 d . . .
H42 H 0.1014 0.2959 0.1312 0.039 Uiso 1 1 calc R . .
C43 C 0.10424(13) 0.1880(10) 0.2352(4) 0.0314(17) Uani 1 1 d . . .
H43 H 0.0880 0.1943 0.2401 0.038 Uiso 1 1 calc R . .
C44 C 0.12076(13) 0.1186(10) 0.2941(4) 0.0265(16) Uani 1 1 d . . .
C45 C 0.12102(14) -0.0263(10) 0.4122(5) 0.0317(18) Uani 1 1 d . . .
C46 C 0.10736(14) -0.0760(10) 0.4750(5) 0.0349(18) Uani 1 1 d . . .
H46A H 0.1064 -0.2058 0.4784 0.052 Uiso 1 1 calc R . .
H46B H 0.0914 -0.0262 0.4651 0.052 Uiso 1 1 calc R . .
H46C H 0.1154 -0.0282 0.5218 0.052 Uiso 1 1 calc R . .
C47 C 0.18841(15) -0.0935(14) 0.5305(5) 0.048(2) Uani 1 1 d . . .
H47A H 0.1723 -0.1235 0.5406 0.058 Uiso 1 1 calc R . .
H47B H 0.1920 0.0313 0.5454 0.058 Uiso 1 1 calc R . .
C48 C 0.20617(17) -0.2169(13) 0.5702(5) 0.049(2) Uani 1 1 d . . .
H48A H 0.2115 -0.1746 0.6212 0.058 Uiso 1 1 calc R . .
H48B H 0.1996 -0.3381 0.5725 0.058 Uiso 1 1 calc R . .
C49 C 0.22538(16) -0.2149(14) 0.5259(6) 0.053(3) Uani 1 1 d . . .
H49A H 0.2343 -0.3281 0.5313 0.064 Uiso 1 1 calc R . .
H49B H 0.2364 -0.1156 0.5410 0.064 Uiso 1 1 calc R . .
C50 C 0.21345(16) -0.1903(13) 0.4470(5) 0.042(2) Uani 1 1 d . . .
H50A H 0.2224 -0.1060 0.4199 0.050 Uiso 1 1 calc R . .
H50B H 0.2122 -0.3052 0.4202 0.050 Uiso 1 1 calc R . .
C51 C 0.23327(12) 0.2942(8) 0.3246(4) 0.0205(15) Uani 1 1 d . . .
C52 C 0.23589(13) 0.3690(9) 0.2576(4) 0.0265(16) Uani 1 1 d . . .
H52 H 0.2227 0.4229 0.2284 0.032 Uiso 1 1 calc R . .
C53 C 0.25739(13) 0.3664(10) 0.2325(4) 0.0288(16) Uani 1 1 d . . .
H53 H 0.2588 0.4163 0.1854 0.035 Uiso 1 1 calc R . .
C54 C 0.27702(13) 0.2923(9) 0.2746(4) 0.0258(16) Uani 1 1 d . . .
C55 C 0.27456(12) 0.2193(10) 0.3428(4) 0.0275(17) Uani 1 1 d . . .
H55 H 0.2878 0.1675 0.3723 0.033 Uiso 1 1 calc R . .
C56 C 0.25284(12) 0.2209(10) 0.3685(4) 0.0262(16) Uani 1 1 d . . .
H56 H 0.2513 0.1722 0.4158 0.031 Uiso 1 1 calc R . .
C57 C 0.30029(13) 0.2906(10) 0.2474(5) 0.0329(18) Uani 1 1 d . . .
H57A H 0.3117 0.2259 0.2828 0.049 Uiso 1 1 calc R . .
H57B H 0.3057 0.4130 0.2426 0.049 Uiso 1 1 calc R . .
H57C H 0.2988 0.2317 0.1990 0.049 Uiso 1 1 calc R . .
C58 C 0.11102(13) 0.4763(9) 0.4143(4) 0.0264(16) Uani 1 1 d . . .
C59 C 0.10365(12) 0.4174(9) 0.4815(4) 0.0270(16) Uani 1 1 d . . .
H59 H 0.0874 0.4245 0.4869 0.032 Uiso 1 1 calc R . .
C60 C 0.11936(14) 0.3502(10) 0.5389(4) 0.0318(17) Uani 1 1 d . . .
H60 H 0.1139 0.3117 0.5832 0.038 Uiso 1 1 calc R . .
C61 C 0.14350(15) 0.3382(10) 0.5325(5) 0.0326(17) Uani 1 1 d . . .
H61 H 0.1544 0.2896 0.5715 0.039 Uiso 1 1 calc R . .
C62 C 0.15103(13) 0.3992(9) 0.4676(4) 0.0305(16) Uani 1 1 d . . .
H62 H 0.1673 0.3937 0.4626 0.037 Uiso 1 1 calc R . .
C63 C 0.13520(14) 0.4675(9) 0.4105(4) 0.0250(16) Uani 1 1 d . . .
C64 C 0.13467(12) 0.6224(10) 0.2918(4) 0.0282(16) Uani 1 1 d . . .
C65 C 0.14916(12) 0.6728(10) 0.2335(4) 0.0300(17) Uani 1 1 d . . .
H65A H 0.1458 0.5917 0.1912 0.045 Uiso 1 1 calc R . .
H65B H 0.1659 0.6651 0.2537 0.045 Uiso 1 1 calc R . .
H65C H 0.1454 0.7948 0.2171 0.045 Uiso 1 1 calc R . .
C66 C 0.06828(15) 0.7293(14) 0.1752(5) 0.057(2) Uani 1 1 d . . .
H66A H 0.0689 0.6122 0.1507 0.068 Uiso 1 1 calc R . .
H66B H 0.0834 0.7911 0.1735 0.068 Uiso 1 1 calc R . .
C67 C 0.0485(2) 0.8366(19) 0.1370(6) 0.096(5) Uani 1 1 d . . .
H67A H 0.0534 0.9621 0.1327 0.115 Uiso 1 1 calc R . .
H67B H 0.0432 0.7893 0.0867 0.115 Uiso 1 1 calc R . .
C68 C 0.02993(16) 0.8225(17) 0.1828(5) 0.068(3) Uani 1 1 d . . .
H68A H 0.0183 0.7318 0.1622 0.082 Uiso 1 1 calc R . .
H68B H 0.0217 0.9379 0.1842 0.082 Uiso 1 1 calc R . .
C69 C 0.04072(14) 0.7711(12) 0.2583(5) 0.037(2) Uani 1 1 d . . .
H69A H 0.0417 0.8747 0.2922 0.044 Uiso 1 1 calc R . .
H69B H 0.0314 0.6765 0.2783 0.044 Uiso 1 1 calc R . .
C70 C 0.02207(12) 0.2844(9) 0.3757(4) 0.0228(15) Uani 1 1 d . . .
C71 C 0.01960(11) 0.3536(9) 0.4478(3) 0.0253(14) Uani 1 1 d . . .
H71 H 0.0326 0.4036 0.4790 0.030 Uiso 1 1 calc R . .
C72 C -0.00258(11) 0.3445(8) 0.4700(4) 0.0263(14) Uani 1 1 d . . .
H72 H -0.0048 0.3912 0.5171 0.032 Uiso 1 1 calc R . .
C73 C -0.02171(12) 0.2684(8) 0.4251(4) 0.0218(14) Uani 1 1 d . . .
C74 C -0.01843(12) 0.2093(9) 0.3556(4) 0.0227(14) Uani 1 1 d . . .
H74 H -0.0315 0.1628 0.3233 0.027 Uiso 1 1 calc R . .
C75 C 0.00349(12) 0.2161(8) 0.3315(4) 0.0238(14) Uani 1 1 d . . .
H75 H 0.0054 0.1725 0.2837 0.029 Uiso 1 1 calc R . .
C76 C -0.04555(13) 0.2597(10) 0.4513(4) 0.0299(16) Uani 1 1 d . . .
H76A H -0.0568 0.1998 0.4138 0.045 Uiso 1 1 calc R . .
H76B H -0.0511 0.3805 0.4592 0.045 Uiso 1 1 calc R . .
H76C H -0.0442 0.1933 0.4980 0.045 Uiso 1 1 calc R . .
N1 N 0.36147(12) 0.0025(7) 0.6031(4) 0.0277(15) Uani 1 1 d . . .
H1 H 0.3467 0.0305 0.6050 0.033 Uiso 1 1 calc R . .
N2 N 0.39481(11) 0.4678(7) 0.5991(3) 0.0212(13) Uani 1 1 d . . .
H2 H 0.4096 0.4368 0.5981 0.025 Uiso 1 1 calc R . .
N3 N 0.11109(12) 0.0647(8) 0.3581(4) 0.0303(15) Uani 1 1 d . . .
H3 H 0.0965 0.0984 0.3605 0.036 Uiso 1 1 calc R . .
N4 N 0.14514(11) 0.5250(7) 0.3481(3) 0.0249(13) Uani 1 1 d . . .
H4 H 0.1598 0.4932 0.3461 0.030 Uiso 1 1 calc R . .
O1 O 0.39269(9) -0.1361(7) 0.6667(3) 0.0286(12) Uani 1 1 d . . .
O2 O 0.44113(9) -0.1536(7) 0.7068(3) 0.0336(12) Uani 1 1 d . . .
O3 O 0.44658(9) 0.0768(6) 0.5765(3) 0.0214(11) Uani 1 1 d . . .
O4 O 0.46019(10) 0.2411(8) 0.6895(3) 0.0285(12) Uani 1 1 d . . .
O5 O 0.44235(9) 0.3973(6) 0.5779(3) 0.0275(12) Uani 1 1 d . . .
O6 O 0.36249(9) 0.6117(7) 0.5332(3) 0.0283(12) Uani 1 1 d . . .
O7 O 0.31429(9) 0.6358(7) 0.4944(3) 0.0323(12) Uani 1 1 d . . .
O8 O 0.30892(9) 0.3938(7) 0.6223(3) 0.0266(12) Uani 1 1 d . . .
O9 O 0.29531(10) 0.2290(8) 0.5101(3) 0.0314(13) Uani 1 1 d . . .
O10 O 0.31310(9) 0.0729(6) 0.6225(3) 0.0259(12) Uani 1 1 d . . .
O11 O 0.14185(9) -0.0844(7) 0.4198(3) 0.0309(12) Uani 1 1 d . . .
O12 O 0.19057(9) -0.1209(8) 0.4536(3) 0.0388(14) Uani 1 1 d . . .
O13 O 0.19571(9) 0.1158(7) 0.3257(3) 0.0236(11) Uani 1 1 d . . .
O14 O 0.19243(10) 0.4386(7) 0.3245(3) 0.0327(14) Uani 1 1 d . . .
O15 O 0.20957(10) 0.2901(8) 0.4359(3) 0.0332(14) Uani 1 1 d . . .
O16 O 0.11342(8) 0.6749(7) 0.2848(3) 0.0282(11) Uani 1 1 d . . .
O17 O 0.06427(9) 0.7067(8) 0.2503(3) 0.0498(16) Uani 1 1 d . . .
O18 O 0.05981(10) 0.4676(7) 0.3776(3) 0.0294(12) Uani 1 1 d . . .
O19 O 0.04574(10) 0.2935(8) 0.2656(3) 0.0374(15) Uani 1 1 d . . .
O20 O 0.06325(9) 0.1486(8) 0.3762(3) 0.0359(14) Uani 1 1 d . . .
Pd1 Pd 0.417901(8) -0.03054(7) 0.61716(2) 0.01620(12) Uani 0.94 1 d P . .
Pd2 Pd 0.337558(9) 0.50448(7) 0.58289(3) 0.01891(13) Uani 0.95 1 d P . .
Pd3 Pd 0.167254(10) 0.01538(8) 0.36798(3) 0.02073(14) Uani 0.90 1 d P . .
Pd4 Pd 0.088223(10) 0.57446(7) 0.33611(3) 0.02069(14) Uani 0.88 1 d P . .
Pd1B Pd 0.4178(3) 0.5138(12) 0.6249(9) 0.053(4) Uani 0.06 1 d P . .
Pd2B Pd 0.3380(3) -0.0482(14) 0.5816(8) 0.022(2) Uani 0.05 1 d P . .
Pd3B Pd 0.16803(13) 0.5340(7) 0.3749(4) 0.0234(15) Uani 0.10 1 d P . .
Pd4B Pd 0.08879(10) -0.0186(5) 0.3374(3) 0.0195(10) Uani 0.12 1 d P . .
S1 S 0.45607(3) 0.2475(2) 0.60961(9) 0.0187(3) Uani 1 1 d . . .
S2 S 0.29949(3) 0.2247(2) 0.59061(10) 0.0214(4) Uani 1 1 d . . .
S3 S 0.20574(3) 0.2877(2) 0.35665(10) 0.0225(4) Uani 1 1 d . . .
S4 S 0.04976(3) 0.2976(2) 0.34557(10) 0.0242(4) 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'
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'
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
_geom_angle_publ_flag
C6 C1 C2 116.6(7) . . ?
C6 C1 Pd1 122.1(5) . . ?
C2 C1 Pd1 121.3(6) . . ?
C3 C2 C1 121.4(7) . . ?
C4 C3 C2 120.6(7) . . ?
C5 C4 C3 119.8(7) . . ?
C4 C5 C6 119.4(7) . . ?
C5 C6 C1 122.2(6) . . ?
C5 C6 N1 116.1(7) . . ?
C1 C6 N1 121.7(7) . . ?
O1 C7 N1 125.0(7) . . ?
O1 C7 C8 117.5(7) . . ?
N1 C7 C8 117.4(7) . . ?
O2 C9 C10 101.6(6) . . ?
C11 C10 C9 102.6(6) . . ?
C10 C11 C12 104.0(6) . . ?
O2 C12 C11 103.6(6) . . ?
C18 C13 C14 120.8(6) . . ?
C18 C13 S1 119.4(5) . . ?
C14 C13 S1 119.8(5) . . ?
C13 C14 C15 118.9(6) . . ?
C16 C15 C14 121.4(7) . . ?
C15 C16 C17 118.5(6) . . ?
C15 C16 C19 121.6(7) . . ?
C17 C16 C19 119.8(6) . . ?
C18 C17 C16 121.6(6) . . ?
C13 C18 C17 118.8(6) . . ?
C25 C20 C21 116.5(7) . . ?
C25 C20 Pd2 122.6(5) . . ?
C21 C20 Pd2 120.7(5) . . ?
C22 C21 C20 122.0(7) . . ?
C21 C22 C23 119.6(7) . . ?
C22 C23 C24 119.8(8) . . ?
C25 C24 C23 119.6(7) . . ?
C24 C25 C20 122.3(7) . . ?
C24 C25 N2 113.8(7) . . ?
C20 C25 N2 123.8(7) . . ?
O6 C26 N2 123.7(6) . . ?
O6 C26 C27 118.2(7) . . ?
N2 C26 C27 118.1(6) . . ?
O7 C28 C29 105.2(7) . . ?
C28 C29 C30 101.2(7) . . ?
C31 C30 C29 104.3(7) . . ?
O7 C31 C30 106.9(7) . . ?
C33 C32 C37 119.6(6) . . ?
C33 C32 S2 121.0(5) . . ?
C37 C32 S2 119.4(5) . . ?
C34 C33 C32 121.1(7) . . ?
C33 C34 C35 120.3(7) . . ?
C36 C35 C34 118.5(6) . . ?
C36 C35 C38 121.5(7) . . ?
C34 C35 C38 120.0(7) . . ?
C37 C36 C35 122.0(7) . . ?
C36 C37 C32 118.6(7) . . ?
C44 C39 C40 118.8(7) . . ?
C44 C39 Pd3 121.0(5) . . ?
C40 C39 Pd3 120.1(6) . . ?
C41 C40 C39 120.9(7) . . ?
C40 C41 C42 120.9(6) . . ?
C41 C42 C43 119.2(7) . . ?
C42 C43 C44 119.4(7) . . ?
C39 C44 N3 124.0(7) . . ?
C39 C44 C43 120.6(6) . . ?
N3 C44 C43 115.3(7) . . ?
O11 C45 N3 126.0(7) . . ?
O11 C45 C46 114.4(7) . . ?
N3 C45 C46 119.6(7) . . ?
O12 C47 C48 103.7(7) . . ?
C49 C48 C47 104.2(8) . . ?
C48 C49 C50 104.5(8) . . ?
O12 C50 C49 105.2(7) . . ?
C52 C51 C56 119.5(6) . . ?
C52 C51 S3 121.5(6) . . ?
C56 C51 S3 119.0(5) . . ?
C51 C52 C53 120.4(7) . . ?
C52 C53 C54 121.1(7) . . ?
C55 C54 C53 118.6(6) . . ?
C55 C54 C57 120.4(7) . . ?
C53 C54 C57 121.0(7) . . ?
C54 C55 C56 120.6(7) . . ?
C55 C56 C51 119.7(7) . . ?
C63 C58 C59 116.4(7) . . ?
C63 C58 Pd4 123.5(5) . . ?
C59 C58 Pd4 120.0(5) . . ?
C60 C59 C58 121.8(7) . . ?
C59 C60 C61 120.4(6) . . ?
C62 C61 C60 118.4(7) . . ?
C63 C62 C61 120.8(7) . . ?
C62 C63 C58 122.1(6) . . ?
C62 C63 N4 115.1(7) . . ?
C58 C63 N4 122.8(7) . . ?
O16 C64 N4 124.7(6) . . ?
O16 C64 C65 118.3(6) . . ?
N4 C64 C65 117.0(6) . . ?
O17 C66 C67 107.4(7) . . ?
C68 C67 C66 105.4(8) . . ?
C67 C68 C69 108.0(8) . . ?
O17 C69 C68 105.4(7) . . ?
C75 C70 C71 120.9(6) . . ?
C75 C70 S4 120.7(5) . . ?
C71 C70 S4 118.4(5) . . ?
C72 C71 C70 117.4(6) . . ?
C71 C72 C73 121.7(6) . . ?
C74 C73 C72 118.2(6) . . ?
C74 C73 C76 121.5(6) . . ?
C72 C73 C76 120.2(6) . . ?
C73 C74 C75 121.6(6) . . ?
C70 C75 C74 120.1(6) . . ?
C7 N1 C6 128.3(7) . . ?
C26 N2 C25 126.2(6) . . ?
C45 N3 C44 127.5(7) . . ?
C64 N4 C63 126.9(6) . . ?
C7 O1 Pd1 126.3(5) . . ?
C12 O2 C9 110.8(6) . . ?
C12 O2 Pd1 126.4(5) . . ?
C9 O2 Pd1 117.1(4) . . ?
S1 O3 Pd1 117.2(3) . . ?
S1 O5 Pd1B 124.0(5) . . ?
C26 O6 Pd2 126.2(5) . . ?
C28 O7 C31 109.3(6) . . ?
C28 O7 Pd2 120.1(5) . . ?
C31 O7 Pd2 125.7(5) . . ?
S2 O8 Pd2 118.7(3) . . ?
C45 O11 Pd3 124.2(5) . . ?
C50 O12 C47 109.8(6) . . ?
C50 O12 Pd3 126.3(5) . . ?
C47 O12 Pd3 120.3(5) . . ?
S3 O13 Pd3 117.6(3) . . ?
S3 O14 Pd3B 118.6(4) . . ?
C64 O16 Pd4 126.0(5) . . ?
C66 O17 C69 109.3(6) . . ?
C66 O17 Pd4 124.9(5) . . ?
C69 O17 Pd4 125.5(5) . . ?
S4 O18 Pd4 118.4(3) . . ?
S4 O20 Pd4B 134.0(4) . . ?
C1 Pd1 O1 92.2(3) . . ?
C1 Pd1 O3 93.8(3) . . ?
O1 Pd1 O3 173.7(2) . . ?
C1 Pd1 O2 174.9(3) . . ?
O1 Pd1 O2 84.0(2) . . ?
O3 Pd1 O2 90.1(2) . . ?
C20 Pd2 O6 92.4(3) . . ?
C20 Pd2 O8 94.2(3) . . ?
O6 Pd2 O8 173.0(2) . . ?
C20 Pd2 O7 173.7(3) . . ?
O6 Pd2 O7 83.3(2) . . ?
O8 Pd2 O7 90.4(2) . . ?
C39 Pd3 O11 92.1(3) . . ?
C39 Pd3 O13 93.8(3) . . ?
O11 Pd3 O13 173.7(2) . . ?
C39 Pd3 O12 173.4(3) . . ?
O11 Pd3 O12 84.2(2) . . ?
O13 Pd3 O12 90.1(2) . . ?
C58 Pd4 O16 91.8(2) . . ?
C58 Pd4 O18 93.9(3) . . ?
O16 Pd4 O18 173.5(2) . . ?
C58 Pd4 O17 174.9(3) . . ?
O16 Pd4 O17 85.1(2) . . ?
O18 Pd4 O17 89.4(2) . . ?
C58 Pd4 Pd4B 111.7(2) . 1_565 ?
O16 Pd4 Pd4B 67.27(17) . 1_565 ?
O18 Pd4 Pd4B 113.37(18) . 1_565 ?
O17 Pd4 Pd4B 63.4(2) . 1_565 ?
O14 Pd3B S3 25.93(19) . . ?
O20 Pd4B Pd4 126.0(2) . 1_545 ?
O4 S1 O5 115.6(3) . . ?
O4 S1 O3 112.2(3) . . ?
O5 S1 O3 111.3(3) . . ?
O4 S1 C13 107.8(3) . . ?
O5 S1 C13 106.6(3) . . ?
O3 S1 C13 102.1(3) . . ?
O9 S2 O10 115.0(3) . . ?
O9 S2 O8 112.2(3) . . ?
O10 S2 O8 112.1(3) . . ?
O9 S2 C32 107.2(3) . . ?
O10 S2 C32 106.8(3) . . ?
O8 S2 C32 102.5(3) . . ?
O15 S3 O14 113.4(4) . . ?
O15 S3 O13 112.8(3) . . ?
O14 S3 O13 112.0(3) . . ?
O15 S3 C51 108.5(3) . . ?
O14 S3 C51 106.9(3) . . ?
O13 S3 C51 102.4(3) . . ?
O15 S3 Pd3B 83.5(3) . . ?
O14 S3 Pd3B 35.5(3) . . ?
O13 S3 Pd3B 110.1(2) . . ?
C51 S3 Pd3B 137.6(3) . . ?
O20 S4 O19 112.2(4) . . ?
O20 S4 O18 111.3(4) . . ?
O19 S4 O18 114.3(4) . . ?
O20 S4 C70 107.3(3) . . ?
O19 S4 C70 107.0(3) . . ?
O18 S4 C70 104.1(3) . . ?
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
C1 C6 1.405(11) . ?
C1 C2 1.412(10) . ?
C1 Pd1 1.943(8) . ?
C2 C3 1.391(11) . ?
C3 C4 1.387(10) . ?
C4 C5 1.387(10) . ?
C5 C6 1.404(11) . ?
C6 N1 1.429(10) . ?
C7 O1 1.232(9) . ?
C7 N1 1.301(10) . ?
C7 C8 1.507(9) . ?
C9 O2 1.473(8) . ?
C9 C10 1.516(10) . ?
C10 C11 1.473(11) . ?
C11 C12 1.542(12) . ?
C12 O2 1.443(9) . ?
C13 C18 1.381(9) . ?
C13 C14 1.385(9) . ?
C13 S1 1.759(6) . ?
C14 C15 1.400(9) . ?
C15 C16 1.362(10) . ?
C16 C17 1.393(10) . ?
C16 C19 1.488(9) . ?
C17 C18 1.384(8) . ?
C20 C25 1.392(10) . ?
C20 C21 1.398(10) . ?
C20 Pd2 1.949(8) . ?
C21 C22 1.380(11) . ?
C22 C23 1.384(11) . ?
C23 C24 1.386(11) . ?
C24 C25 1.376(11) . ?
C25 N2 1.414(9) . ?
C26 O6 1.281(8) . ?
C26 N2 1.357(10) . ?
C26 C27 1.469(9) . ?
C28 O7 1.425(10) . ?
C28 C29 1.502(12) . ?
C29 C30 1.548(12) . ?
C30 C31 1.474(13) . ?
C31 O7 1.453(10) . ?
C32 C33 1.375(10) . ?
C32 C37 1.415(9) . ?
C32 S2 1.752(6) . ?
C33 C34 1.362(10) . ?
C34 C35 1.410(10) . ?
C35 C36 1.377(11) . ?
C35 C38 1.504(9) . ?
C36 C37 1.375(9) . ?
C39 C44 1.379(10) . ?
C39 C40 1.399(9) . ?
C39 Pd3 1.955(8) . ?
C40 C41 1.379(11) . ?
C41 C42 1.389(10) . ?
C42 C43 1.393(10) . ?
C43 C44 1.426(11) . ?
C44 N3 1.418(9) . ?
C45 O11 1.260(9) . ?
C45 N3 1.266(10) . ?
C45 C46 1.520(10) . ?
C47 O12 1.438(10) . ?
C47 C48 1.487(12) . ?
C48 C49 1.453(13) . ?
C49 C50 1.513(13) . ?
C50 O12 1.432(10) . ?
C51 C52 1.370(10) . ?
C51 C56 1.396(10) . ?
C51 S3 1.758(7) . ?
C52 C53 1.374(9) . ?
C53 C54 1.386(11) . ?
C54 C55 1.382(11) . ?
C54 C57 1.486(10) . ?
C55 C56 1.391(9) . ?
C58 C63 1.399(10) . ?
C58 C59 1.419(10) . ?
C58 Pd4 1.938(8) . ?
C59 C60 1.376(11) . ?
C60 C61 1.407(11) . ?
C61 C62 1.391(10) . ?
C62 C63 1.379(11) . ?
C63 N4 1.408(9) . ?
C64 O16 1.269(8) . ?
C64 N4 1.333(10) . ?
C64 C65 1.486(9) . ?
C66 O17 1.428(9) . ?
C66 C67 1.481(12) . ?
C67 C68 1.446(13) . ?
C68 C69 1.477(12) . ?
C69 O17 1.460(9) . ?
C70 C75 1.343(9) . ?
C70 C71 1.437(9) . ?
C70 S4 1.753(7) . ?
C71 C72 1.389(8) . ?
C72 C73 1.395(10) . ?
C73 C74 1.379(9) . ?
C73 C76 1.511(9) . ?
C74 C75 1.389(9) . ?
O1 Pd1 1.975(5) . ?
O2 Pd1 2.164(6) . ?
O3 S1 1.488(5) . ?
O3 Pd1 2.060(5) . ?
O4 S1 1.440(5) . ?
O5 S1 1.447(5) . ?
O5 Pd1B 1.954(17) . ?
O6 Pd2 1.968(5) . ?
O7 Pd2 2.178(5) . ?
O8 S2 1.468(6) . ?
O8 Pd2 2.057(5) . ?
O9 S2 1.452(6) . ?
O10 S2 1.456(5) . ?
O11 Pd3 1.989(5) . ?
O12 Pd3 2.163(6) . ?
O13 S3 1.493(5) . ?
O13 Pd3 2.044(5) . ?
O14 S3 1.445(6) . ?
O14 Pd3B 1.917(8) . ?
O15 S3 1.428(6) . ?
O16 Pd4 1.977(5) . ?
O17 Pd4 2.170(5) . ?
O18 S4 1.488(6) . ?
O18 Pd4 2.053(5) . ?
O19 S4 1.442(6) . ?
O20 S4 1.429(6) . ?
O20 Pd4B 2.125(7) . ?
Pd4 Pd4B 3.061(4) 1_565 ?
Pd3B S3 2.901(7) . ?
Pd4B Pd4 3.061(4) 1_545 ?
