# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

loop_
_publ_author_name
'Jason Love'
'Claire Wilson'
'Alexander J. Blake'
'Gonzalo Givaja'
'Martin Schroder'

_publ_contact_author_name        'Dr Jason Love'
_publ_contact_author_address     
;
Nottingham
UNITED KINGDOM
;

_publ_contact_author_email       JASON.LOVE@NOTTINGHAM.AC.UK

_publ_section_title              
;
Macrocyclic diiminodipyrromethane complexes:
structural analogues of Pac-Man porphyrins
;

data_PDBZPY
_database_code_CSD               216097

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H40 N8 Pd2, 0.5(C4 H10 O)'
_chemical_formula_sum            'C60 H45 N8 O0.50 Pd2'
_chemical_formula_weight         1098.84

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'
Pd Pd -0.9988 1.0072 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3192(14)
_cell_length_b                   13.238(2)
_cell_length_c                   18.403(2)
_cell_angle_alpha                84.446(2)
_cell_angle_beta                 77.151(2)
_cell_angle_gamma                75.866(2)
_cell_volume                     2374.4(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9886
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.5

_exptl_crystal_description       tablet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1114
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   '(SADABS version 2.03; Bruker, 2001)'

_exptl_special_details           
;
Et2O solvent of crystallisation: geometric restraints applied,
isotropic model
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20521
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.044
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         27.50
_reflns_number_total             10455
_reflns_number_gt                8190
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  
'SHELXL-97; enCIFer (CCDC, 2003); PLATON (Spek, 2003)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10454
_refine_ls_number_parameters     633
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0964
_refine_ls_wR_factor_gt          0.0886
_refine_ls_goodness_of_fit_ref   0.98
_refine_ls_restrained_S_all      0.98
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 -0.25338(2) -0.050412(16) 0.382450(11) 0.01711(7) Uani 1 1 d . . .
Pd2 Pd -0.04413(2) -0.331719(16) 0.362597(11) 0.01684(7) Uani 1 1 d . . .
N1 N -0.4261(2) -0.10206(19) 0.38217(13) 0.0198(5) Uani 1 1 d . . .
N2 N -0.3033(2) 0.02219(18) 0.29209(13) 0.0201(5) Uani 1 1 d . . .
N3 N -0.0879(2) 0.00206(18) 0.35841(13) 0.0184(5) Uani 1 1 d . . .
N4 N -0.1608(2) -0.12336(18) 0.47051(13) 0.0188(5) Uani 1 1 d . . .
N5 N -0.0167(2) -0.33412(18) 0.47021(13) 0.0189(5) Uani 1 1 d . . .
N6 N 0.1527(2) -0.36168(19) 0.34401(13) 0.0192(5) Uani 1 1 d . . .
N7 N -0.0310(2) -0.32228(19) 0.25543(13) 0.0203(5) Uani 1 1 d . . .
N8 N -0.2503(2) -0.29892(18) 0.36032(13) 0.0188(5) Uani 1 1 d . . .
C1 C -0.4756(3) -0.0701(2) 0.32220(16) 0.0213(6) Uani 1 1 d . . .
H1A H -0.5511 -0.0925 0.3132 0.026 Uiso 1 1 calc R . .
C2 C -0.4118(3) -0.0004(2) 0.27103(17) 0.0221(6) Uani 1 1 d . . .
C3 C -0.4138(3) 0.0403(2) 0.19760(17) 0.0272(7) Uani 1 1 d . . .
H3A H -0.4788 0.0375 0.1689 0.033 Uiso 1 1 calc R . .
C4 C -0.3020(3) 0.0853(2) 0.17529(17) 0.0273(7) Uani 1 1 d . . .
H4A H -0.2760 0.1188 0.1281 0.033 Uiso 1 1 calc R . .
C5 C -0.2340(3) 0.0725(2) 0.23529(16) 0.0209(6) Uani 1 1 d . . .
C6 C -0.1105(3) 0.1139(2) 0.24045(15) 0.0200(6) Uani 1 1 d . . .
C7 C -0.0170(3) 0.1054(2) 0.16179(15) 0.0220(6) Uani 1 1 d . . .
C8 C 0.0372(4) 0.0068(3) 0.13387(18) 0.0339(8) Uani 1 1 d . . .
H8A H 0.0200 -0.0529 0.1640 0.041 Uiso 1 1 calc R . .
C9 C 0.1168(4) -0.0053(3) 0.06184(19) 0.0395(9) Uani 1 1 d . . .
H9A H 0.1533 -0.0730 0.0431 0.047 Uiso 1 1 calc R . .
C10 C 0.1424(4) 0.0809(3) 0.01797(18) 0.0381(8) Uani 1 1 d . . .
H10A H 0.1966 0.0726 -0.0310 0.046 Uiso 1 1 calc R . .
C11 C 0.0894(4) 0.1789(3) 0.04514(17) 0.0354(8) Uani 1 1 d . . .
H11A H 0.1079 0.2383 0.0151 0.043 Uiso 1 1 calc R . .
C12 C 0.0082(3) 0.1914(2) 0.11719(16) 0.0264(7) Uani 1 1 d . . .
H12A H -0.0297 0.2593 0.1354 0.032 Uiso 1 1 calc R . .
C13 C -0.1602(3) 0.2288(2) 0.26469(15) 0.0199(6) Uani 1 1 d . . .
C14 C -0.2906(3) 0.2861(2) 0.26098(17) 0.0260(7) Uani 1 1 d . . .
H14A H -0.3511 0.2542 0.2442 0.031 Uiso 1 1 calc R . .
C15 C -0.3347(3) 0.3898(3) 0.28149(18) 0.0321(7) Uani 1 1 d . . .
H15A H -0.4250 0.4272 0.2793 0.039 Uiso 1 1 calc R . .
C16 C -0.2478(4) 0.4379(3) 0.30481(17) 0.0308(7) Uani 1 1 d . . .
H16A H -0.2770 0.5089 0.3177 0.037 Uiso 1 1 calc R . .
C17 C -0.1177(3) 0.3819(3) 0.30927(18) 0.0307(7) Uani 1 1 d . . .
H17A H -0.0573 0.4144 0.3256 0.037 Uiso 1 1 calc R . .
C18 C -0.0749(3) 0.2784(2) 0.28993(17) 0.0278(7) Uani 1 1 d . . .
H18A H 0.0143 0.2406 0.2940 0.033 Uiso 1 1 calc R . .
C19 C -0.0287(3) 0.0512(2) 0.29685(15) 0.0207(6) Uani 1 1 d . . .
C20 C 0.1088(3) 0.0414(2) 0.30092(17) 0.0252(7) Uani 1 1 d . . .
H20A H 0.1744 0.0694 0.2654 0.030 Uiso 1 1 calc R . .
C21 C 0.1315(3) -0.0165(2) 0.36588(16) 0.0246(6) Uani 1 1 d . . .
H21A H 0.2148 -0.0352 0.3831 0.030 Uiso 1 1 calc R . .
C22 C 0.0080(3) -0.0415(2) 0.40087(16) 0.0205(6) Uani 1 1 d . . .
C23 C -0.0383(3) -0.1073(2) 0.46139(15) 0.0203(6) Uani 1 1 d . . .
H23A H 0.0192 -0.1394 0.4949 0.024 Uiso 1 1 calc R . .
C24 C -0.2008(3) -0.1965(2) 0.52952(15) 0.0188(6) Uani 1 1 d . . .
C25 C -0.3168(3) -0.1645(2) 0.58500(16) 0.0227(6) Uani 1 1 d . . .
H25A H -0.3719 -0.0959 0.5823 0.027 Uiso 1 1 calc R . .
C26 C -0.3521(3) -0.2327(3) 0.64415(16) 0.0261(7) Uani 1 1 d . . .
H26A H -0.4306 -0.2104 0.6821 0.031 Uiso 1 1 calc R . .
C27 C -0.2727(3) -0.3334(2) 0.64803(16) 0.0260(7) Uani 1 1 d . . .
H27A H -0.2954 -0.3791 0.6895 0.031 Uiso 1 1 calc R . .
C28 C -0.1605(3) -0.3677(2) 0.59187(16) 0.0221(6) Uani 1 1 d . . .
H28A H -0.1084 -0.4374 0.5936 0.027 Uiso 1 1 calc R . .
C29 C -0.1244(3) -0.2989(2) 0.53258(14) 0.0188(6) Uani 1 1 d . . .
C30 C 0.1123(3) -0.3522(2) 0.47353(16) 0.0213(6) Uani 1 1 d . . .
H30A H 0.1392 -0.3534 0.5198 0.026 Uiso 1 1 calc R . .
C31 C 0.2111(3) -0.3702(2) 0.40583(15) 0.0204(6) Uani 1 1 d . . .
C32 C 0.3512(3) -0.3801(2) 0.38096(17) 0.0257(7) Uani 1 1 d . . .
H32A H 0.4169 -0.3874 0.4111 0.031 Uiso 1 1 calc R . .
C33 C 0.3761(3) -0.3774(2) 0.30352(17) 0.0260(7) Uani 1 1 d . . .
H33A H 0.4627 -0.3828 0.2709 0.031 Uiso 1 1 calc R . .
C34 C 0.2499(3) -0.3651(2) 0.28174(16) 0.0211(6) Uani 1 1 d . . .
C35 C 0.2227(3) -0.3616(2) 0.20259(15) 0.0207(6) Uani 1 1 d . . .
C36 C 0.2679(3) -0.4762(2) 0.17917(15) 0.0209(6) Uani 1 1 d . . .
C37 C 0.1733(3) -0.5348(3) 0.17859(18) 0.0296(7) Uani 1 1 d . . .
H37A H 0.0786 -0.5023 0.1881 0.036 Uiso 1 1 calc R . .
C38 C 0.2152(4) -0.6405(3) 0.16428(19) 0.0365(8) Uani 1 1 d . . .
H38A H 0.1491 -0.6796 0.1648 0.044 Uiso 1 1 calc R . .
C39 C 0.3519(4) -0.6887(3) 0.14943(18) 0.0355(8) Uani 1 1 d . . .
H39A H 0.3803 -0.7608 0.1398 0.043 Uiso 1 1 calc R . .
C40 C 0.4473(4) -0.6313(3) 0.14863(19) 0.0373(8) Uani 1 1 d . . .
H40A H 0.5418 -0.6640 0.1374 0.045 Uiso 1 1 calc R . .
C41 C 0.4067(3) -0.5264(3) 0.16401(18) 0.0319(7) Uani 1 1 d . . .
H41A H 0.4736 -0.4883 0.1643 0.038 Uiso 1 1 calc R . .
C42 C 0.3064(3) -0.2888(3) 0.15262(17) 0.0269(7) Uani 1 1 d . . .
C43 C 0.3757(4) -0.3107(3) 0.0808(2) 0.0498(11) Uani 1 1 d . . .
H43A H 0.3720 -0.3719 0.0591 0.060 Uiso 1 1 calc R . .
C44 C 0.4519(5) -0.2421(4) 0.0400(3) 0.0725(16) Uani 1 1 d . . .
H44A H 0.5015 -0.2583 -0.0091 0.087 Uiso 1 1 calc R . .
C45 C 0.4561(5) -0.1527(4) 0.0693(3) 0.0690(15) Uani 1 1 d . . .
H45A H 0.5102 -0.1079 0.0413 0.083 Uiso 1 1 calc R . .
C46 C 0.3816(5) -0.1276(3) 0.1396(2) 0.0535(11) Uani 1 1 d . . .
H46A H 0.3813 -0.0641 0.1598 0.064 Uiso 1 1 calc R . .
C47 C 0.3072(4) -0.1954(3) 0.1807(2) 0.0374(8) Uani 1 1 d . . .
H47A H 0.2556 -0.1777 0.2292 0.045 Uiso 1 1 calc R . .
C48 C 0.0732(3) -0.3194(2) 0.19740(15) 0.0203(6) Uani 1 1 d . . .
C49 C 0.0173(3) -0.2845(3) 0.13357(17) 0.0294(7) Uani 1 1 d . . .
H49A H 0.0676 -0.2755 0.0844 0.035 Uiso 1 1 calc R . .
C50 C -0.1238(3) -0.2655(3) 0.15512(16) 0.0278(7) Uani 1 1 d . . .
H50A H -0.1881 -0.2417 0.1239 0.033 Uiso 1 1 calc R . .
C51 C -0.1529(3) -0.2885(2) 0.23243(16) 0.0212(6) Uani 1 1 d . . .
C52 C -0.2686(3) -0.2800(2) 0.29133(15) 0.0190(6) Uani 1 1 d . . .
H52A H -0.3581 -0.2611 0.2813 0.023 Uiso 1 1 calc R . .
C53 C -0.3663(3) -0.2848(2) 0.42100(15) 0.0186(6) Uani 1 1 d . . .
C54 C -0.3830(3) -0.3653(2) 0.47399(16) 0.0205(6) Uani 1 1 d . . .
H54A H -0.3169 -0.4296 0.4703 0.025 Uiso 1 1 calc R . .
C55 C -0.4960(3) -0.3519(2) 0.53221(16) 0.0254(7) Uani 1 1 d . . .
H55A H -0.5069 -0.4072 0.5683 0.030 Uiso 1 1 calc R . .
C56 C -0.5934(3) -0.2584(3) 0.53829(16) 0.0259(7) Uani 1 1 d . . .
H56A H -0.6728 -0.2510 0.5769 0.031 Uiso 1 1 calc R . .
C57 C -0.5744(3) -0.1757(2) 0.48769(16) 0.0221(6) Uani 1 1 d . . .
H57A H -0.6389 -0.1106 0.4930 0.026 Uiso 1 1 calc R . .
C58 C -0.4609(3) -0.1884(2) 0.42925(16) 0.0199(6) Uani 1 1 d . . .
C1S C 0.2392(10) 0.4596(9) -0.0445(6) 0.079(3) Uiso 0.50 1 d PD A -1
H1SA H 0.2962 0.4954 -0.0831 0.118 Uiso 0.50 1 calc PR A -1
H1SB H 0.2555 0.3865 -0.0566 0.118 Uiso 0.50 1 calc PR A -1
H1SC H 0.2623 0.4631 0.0039 0.118 Uiso 0.50 1 calc PR A -1
C2S C 0.0957(9) 0.5100(9) -0.0410(6) 0.070(3) Uiso 0.50 1 d PD A -1
H2SA H 0.0796 0.5841 -0.0297 0.084 Uiso 0.50 1 calc PR A -1
H2SB H 0.0726 0.5073 -0.0901 0.084 Uiso 0.50 1 calc PR A -1
O3S O 0.0124(5) 0.4611(4) 0.0133(3) 0.0502(14) Uiso 0.50 1 d PD A -1
C4S C -0.1239(8) 0.5084(9) 0.0191(6) 0.061(3) Uiso 0.50 1 d PD A -1
H4SA H -0.1485 0.5070 -0.0298 0.074 Uiso 0.50 1 calc PR A -1
H4SB H -0.1382 0.5824 0.0304 0.074 Uiso 0.50 1 calc PR A -1
C5S C -0.2142(12) 0.4608(10) 0.0753(7) 0.099(4) Uiso 0.50 1 d PD A -1
H5SA H -0.3089 0.4983 0.0761 0.148 Uiso 0.50 1 calc PR A -1
H5SB H -0.1925 0.4636 0.1242 0.148 Uiso 0.50 1 calc PR A -1
H5SC H -0.2027 0.3879 0.0640 0.148 Uiso 0.50 1 calc PR A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.01765(12) 0.01771(12) 0.01649(11) 0.00176(8) -0.00270(8) -0.00674(8)
Pd2 0.01628(11) 0.02128(12) 0.01292(11) -0.00022(8) -0.00214(8) -0.00521(9)
N1 0.0176(12) 0.0198(12) 0.0214(12) 0.0003(10) -0.0020(10) -0.0057(10)
N2 0.0213(12) 0.0180(12) 0.0222(12) 0.0023(10) -0.0075(10) -0.0050(10)
N3 0.0197(12) 0.0199(12) 0.0168(11) 0.0026(9) -0.0044(9) -0.0075(10)
N4 0.0206(12) 0.0186(12) 0.0176(12) -0.0007(10) -0.0035(10) -0.0056(10)
N5 0.0209(12) 0.0191(12) 0.0169(12) -0.0003(9) -0.0045(10) -0.0047(10)
N6 0.0181(12) 0.0227(13) 0.0177(12) -0.0022(10) -0.0038(9) -0.0056(10)
N7 0.0216(12) 0.0259(13) 0.0141(11) -0.0026(10) -0.0039(9) -0.0061(10)
N8 0.0197(12) 0.0196(12) 0.0171(12) 0.0002(10) -0.0033(9) -0.0052(10)
C1 0.0155(14) 0.0220(15) 0.0262(15) -0.0025(12) -0.0041(12) -0.0037(11)
C2 0.0212(15) 0.0200(15) 0.0257(15) 0.0014(12) -0.0066(12) -0.0054(12)
C3 0.0331(17) 0.0259(16) 0.0288(16) 0.0032(13) -0.0155(14) -0.0119(14)
C4 0.0352(18) 0.0280(17) 0.0226(15) 0.0060(13) -0.0103(13) -0.0136(14)
C5 0.0230(15) 0.0199(15) 0.0206(14) 0.0000(11) -0.0041(12) -0.0072(12)
C6 0.0218(14) 0.0205(15) 0.0183(14) 0.0028(11) -0.0027(11) -0.0088(12)
C7 0.0232(15) 0.0282(16) 0.0160(14) 0.0016(12) -0.0033(11) -0.0101(12)
C8 0.044(2) 0.0300(18) 0.0251(16) 0.0014(14) -0.0015(15) -0.0094(15)
C9 0.050(2) 0.035(2) 0.0284(18) -0.0095(15) 0.0012(16) -0.0045(17)
C10 0.044(2) 0.047(2) 0.0194(16) -0.0036(15) 0.0031(15) -0.0126(17)
C11 0.048(2) 0.039(2) 0.0192(16) 0.0059(14) -0.0006(14) -0.0182(17)
C12 0.0332(17) 0.0274(17) 0.0197(15) 0.0021(13) -0.0024(13) -0.0130(14)
C13 0.0259(15) 0.0202(15) 0.0134(13) 0.0047(11) 0.0009(11) -0.0114(12)
C14 0.0278(16) 0.0250(16) 0.0260(16) 0.0003(13) -0.0054(13) -0.0085(13)
C15 0.0318(18) 0.0271(17) 0.0343(18) -0.0007(14) -0.0055(14) -0.0022(14)
C16 0.045(2) 0.0225(16) 0.0250(16) -0.0008(13) -0.0026(14) -0.0120(14)
C17 0.0373(19) 0.0308(18) 0.0295(17) -0.0028(14) -0.0072(14) -0.0176(15)
C18 0.0295(17) 0.0293(17) 0.0258(16) 0.0005(13) -0.0066(13) -0.0090(13)
C19 0.0217(15) 0.0220(15) 0.0187(14) -0.0006(11) -0.0021(11) -0.0078(12)
C20 0.0211(15) 0.0293(17) 0.0244(15) 0.0035(13) 0.0011(12) -0.0114(13)
C21 0.0228(15) 0.0268(16) 0.0250(15) 0.0004(13) -0.0056(12) -0.0075(12)
C22 0.0206(14) 0.0230(15) 0.0195(14) -0.0014(12) -0.0039(11) -0.0080(12)
C23 0.0270(15) 0.0176(14) 0.0162(13) -0.0012(11) -0.0042(11) -0.0050(12)
C24 0.0231(15) 0.0220(15) 0.0140(13) 0.0017(11) -0.0052(11) -0.0097(12)
C25 0.0257(15) 0.0221(15) 0.0207(14) -0.0033(12) -0.0052(12) -0.0050(12)
C26 0.0254(16) 0.0361(18) 0.0160(14) -0.0023(13) 0.0022(12) -0.0108(13)
C27 0.0350(18) 0.0302(17) 0.0145(14) 0.0055(12) -0.0045(12) -0.0139(14)
C28 0.0260(15) 0.0214(15) 0.0210(15) 0.0027(12) -0.0078(12) -0.0078(12)
C29 0.0215(14) 0.0262(15) 0.0106(12) -0.0005(11) -0.0032(11) -0.0095(12)
C30 0.0250(15) 0.0208(15) 0.0191(14) 0.0011(12) -0.0076(12) -0.0051(12)
C31 0.0224(15) 0.0239(15) 0.0156(13) -0.0029(11) -0.0052(11) -0.0045(12)
C32 0.0213(15) 0.0292(17) 0.0283(16) -0.0052(13) -0.0090(13) -0.0040(13)
C33 0.0172(14) 0.0343(18) 0.0259(16) -0.0076(13) -0.0006(12) -0.0058(13)
C34 0.0206(14) 0.0241(15) 0.0184(14) -0.0046(12) -0.0009(11) -0.0064(12)
C35 0.0189(14) 0.0268(16) 0.0167(14) -0.0031(12) -0.0001(11) -0.0081(12)
C36 0.0231(15) 0.0245(15) 0.0153(13) -0.0032(11) -0.0011(11) -0.0074(12)
C37 0.0229(16) 0.0365(19) 0.0296(17) -0.0069(14) -0.0022(13) -0.0079(14)
C38 0.040(2) 0.034(2) 0.038(2) -0.0079(16) -0.0006(16) -0.0180(16)
C39 0.048(2) 0.0302(18) 0.0247(17) -0.0070(14) -0.0044(15) -0.0032(16)
C40 0.0300(18) 0.043(2) 0.0354(19) -0.0152(16) -0.0038(15) 0.0014(15)
C41 0.0252(17) 0.040(2) 0.0307(17) -0.0124(15) -0.0014(14) -0.0073(14)
C42 0.0256(16) 0.0331(18) 0.0227(15) -0.0004(13) -0.0011(13) -0.0115(13)
C43 0.067(3) 0.050(2) 0.0285(19) -0.0053(17) 0.0149(18) -0.027(2)
C44 0.085(4) 0.068(3) 0.047(3) 0.004(2) 0.034(2) -0.032(3)
C45 0.066(3) 0.075(4) 0.068(3) 0.022(3) 0.006(2) -0.048(3)
C46 0.065(3) 0.051(3) 0.058(3) 0.009(2) -0.017(2) -0.039(2)
C47 0.042(2) 0.040(2) 0.0357(19) 0.0010(16) -0.0075(16) -0.0217(17)
C48 0.0203(14) 0.0238(15) 0.0165(13) -0.0036(11) -0.0011(11) -0.0058(12)
C49 0.0307(17) 0.0381(19) 0.0159(14) 0.0032(13) -0.0002(12) -0.0073(14)
C50 0.0286(17) 0.0357(18) 0.0180(15) 0.0016(13) -0.0074(12) -0.0039(14)
C51 0.0230(15) 0.0225(15) 0.0182(14) -0.0010(12) -0.0065(12) -0.0038(12)
C52 0.0212(14) 0.0175(14) 0.0201(14) 0.0005(11) -0.0063(11) -0.0065(11)
C53 0.0170(14) 0.0246(15) 0.0162(13) -0.0004(11) -0.0037(11) -0.0088(11)
C54 0.0221(15) 0.0207(15) 0.0213(14) -0.0019(12) -0.0069(12) -0.0072(12)
C55 0.0321(17) 0.0308(17) 0.0177(14) 0.0062(12) -0.0066(12) -0.0169(14)
C56 0.0232(15) 0.0394(19) 0.0152(14) -0.0020(13) 0.0022(12) -0.0129(14)
C57 0.0187(14) 0.0228(15) 0.0248(15) -0.0034(12) -0.0019(12) -0.0062(12)
C58 0.0216(14) 0.0200(15) 0.0202(14) 0.0013(11) -0.0043(11) -0.0099(12)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N1 2.060(2) . ?
Pd1 N2 1.945(2) . ?
Pd1 N3 1.944(2) . ?
Pd1 N4 2.099(2) . ?
Pd2 N5 2.058(2) . ?
Pd2 N6 1.929(2) . ?
Pd2 N7 1.940(2) . ?
Pd2 N8 2.074(2) . ?
N1 C1 1.308(4) . ?
N1 C58 1.434(4) . ?
N2 C5 1.346(4) . ?
N2 C2 1.369(4) . ?
N3 C19 1.350(3) . ?
N3 C22 1.379(4) . ?
N4 C23 1.304(4) . ?
N4 C24 1.442(3) . ?
N5 C30 1.308(4) . ?
N5 C29 1.433(3) . ?
N6 C34 1.341(3) . ?
N6 C31 1.385(3) . ?
N7 C48 1.341(3) . ?
N7 C51 1.373(4) . ?
N8 C52 1.316(3) . ?
N8 C53 1.432(3) . ?
C1 C2 1.422(4) . ?
C2 C3 1.408(4) . ?
C3 C4 1.391(4) . ?
C4 C5 1.411(4) . ?
C5 C6 1.529(4) . ?
C6 C19 1.536(4) . ?
C6 C7 1.548(4) . ?
C6 C13 1.557(4) . ?
C7 C12 1.381(4) . ?
C7 C8 1.387(4) . ?
C8 C9 1.396(5) . ?
C9 C10 1.377(5) . ?
C10 C11 1.375(5) . ?
C11 C12 1.403(4) . ?
C13 C14 1.387(4) . ?
C13 C18 1.394(4) . ?
C14 C15 1.398(4) . ?
C15 C16 1.378(5) . ?
C16 C17 1.382(5) . ?
C17 C18 1.389(4) . ?
C19 C20 1.411(4) . ?
C20 C21 1.389(4) . ?
C21 C22 1.397(4) . ?
C22 C23 1.416(4) . ?
C24 C29 1.395(4) . ?
C24 C25 1.396(4) . ?
C25 C26 1.388(4) . ?
C26 C27 1.389(4) . ?
C27 C28 1.384(4) . ?
C28 C29 1.397(4) . ?
C30 C31 1.422(4) . ?
C31 C32 1.394(4) . ?
C32 C33 1.389(4) . ?
C33 C34 1.413(4) . ?
C34 C35 1.538(4) . ?
C35 C48 1.528(4) . ?
C35 C36 1.548(4) . ?
C35 C42 1.550(4) . ?
C36 C37 1.390(4) . ?
C36 C41 1.402(4) . ?
C37 C38 1.393(5) . ?
C38 C39 1.376(5) . ?
C39 C40 1.379(5) . ?
C40 C41 1.386(5) . ?
C42 C43 1.376(5) . ?
C42 C47 1.388(5) . ?
C43 C44 1.399(5) . ?
C44 C45 1.361(7) . ?
C45 C46 1.376(6) . ?
C46 C47 1.384(5) . ?
C48 C49 1.411(4) . ?
C49 C50 1.387(4) . ?
C50 C51 1.406(4) . ?
C51 C52 1.413(4) . ?
C53 C54 1.389(4) . ?
C53 C58 1.403(4) . ?
C54 C55 1.385(4) . ?
C55 C56 1.386(4) . ?
C56 C57 1.389(4) . ?
C57 C58 1.391(4) . ?
C1S C2S 1.457(10) . ?
C2S O3S 1.386(8) . ?
O3S C4S 1.378(8) . ?
C4S C5S 1.438(10) . ?

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
N3 Pd1 N2 88.42(10) . . ?
N3 Pd1 N1 166.98(9) . . ?
N2 Pd1 N1 79.86(10) . . ?
N3 Pd1 N4 80.48(9) . . ?
N2 Pd1 N4 168.53(9) . . ?
N1 Pd1 N4 110.86(9) . . ?
N6 Pd2 N7 88.17(10) . . ?
N6 Pd2 N5 80.37(9) . . ?
N7 Pd2 N5 167.47(9) . . ?
N6 Pd2 N8 168.92(9) . . ?
N7 Pd2 N8 80.75(9) . . ?
N5 Pd2 N8 110.69(9) . . ?
C1 N1 C58 122.4(2) . . ?
C1 N1 Pd1 112.64(19) . . ?
C58 N1 Pd1 122.20(18) . . ?
C5 N2 C2 109.8(2) . . ?
C5 N2 Pd1 131.8(2) . . ?
C2 N2 Pd1 116.28(19) . . ?
C19 N3 C22 109.3(2) . . ?
C19 N3 Pd1 132.6(2) . . ?
C22 N3 Pd1 115.34(18) . . ?
C23 N4 C24 117.6(2) . . ?
C23 N4 Pd1 110.33(19) . . ?
C24 N4 Pd1 131.40(18) . . ?
C30 N5 C29 122.4(2) . . ?
C30 N5 Pd2 112.31(19) . . ?
C29 N5 Pd2 124.10(18) . . ?
C34 N6 C31 109.5(2) . . ?
C34 N6 Pd2 133.5(2) . . ?
C31 N6 Pd2 116.52(18) . . ?
C48 N7 C51 109.9(2) . . ?
C48 N7 Pd2 132.7(2) . . ?
C51 N7 Pd2 115.46(18) . . ?
C52 N8 C53 119.6(2) . . ?
C52 N8 Pd2 110.64(18) . . ?
C53 N8 Pd2 129.42(18) . . ?
N1 C1 C2 117.3(3) . . ?
N2 C2 C3 108.1(3) . . ?
N2 C2 C1 113.6(3) . . ?
C3 C2 C1 137.4(3) . . ?
C4 C3 C2 106.5(3) . . ?
C3 C4 C5 107.8(3) . . ?
N2 C5 C4 107.8(3) . . ?
N2 C5 C6 123.9(3) . . ?
C4 C5 C6 128.1(3) . . ?
C5 C6 C19 113.4(2) . . ?
C5 C6 C7 106.1(2) . . ?
C19 C6 C7 108.6(2) . . ?
C5 C6 C13 109.2(2) . . ?
C19 C6 C13 107.8(2) . . ?
C7 C6 C13 111.8(2) . . ?
C12 C7 C8 119.1(3) . . ?
C12 C7 C6 122.9(3) . . ?
C8 C7 C6 117.9(3) . . ?
C7 C8 C9 120.5(3) . . ?
C10 C9 C8 120.1(3) . . ?
C11 C10 C9 119.9(3) . . ?
C10 C11 C12 120.1(3) . . ?
C7 C12 C11 120.3(3) . . ?
C14 C13 C18 117.6(3) . . ?
C14 C13 C6 121.1(3) . . ?
C18 C13 C6 121.4(3) . . ?
C13 C14 C15 121.2(3) . . ?
C16 C15 C14 120.3(3) . . ?
C15 C16 C17 119.3(3) . . ?
C16 C17 C18 120.2(3) . . ?
C17 C18 C13 121.4(3) . . ?
N3 C19 C20 107.5(3) . . ?
N3 C19 C6 122.2(2) . . ?
C20 C19 C6 130.0(3) . . ?
C21 C20 C19 108.2(3) . . ?
C20 C21 C22 106.5(3) . . ?
N3 C22 C21 108.4(2) . . ?
N3 C22 C23 113.9(2) . . ?
C21 C22 C23 137.2(3) . . ?
N4 C23 C22 119.2(3) . . ?
C29 C24 C25 119.2(3) . . ?
C29 C24 N4 121.0(2) . . ?
C25 C24 N4 119.8(3) . . ?
C26 C25 C24 120.2(3) . . ?
C25 C26 C27 120.1(3) . . ?
C28 C27 C26 120.4(3) . . ?
C27 C28 C29 119.5(3) . . ?
C24 C29 C28 120.5(3) . . ?
C24 C29 N5 118.3(2) . . ?
C28 C29 N5 121.0(3) . . ?
N5 C30 C31 118.0(3) . . ?
N6 C31 C32 108.2(2) . . ?
N6 C31 C30 112.8(2) . . ?
C32 C31 C30 138.4(3) . . ?
C33 C32 C31 106.7(3) . . ?
C32 C33 C34 108.0(3) . . ?
N6 C34 C33 107.6(2) . . ?
N6 C34 C35 123.8(2) . . ?
C33 C34 C35 128.5(3) . . ?
C48 C35 C34 114.4(2) . . ?
C48 C35 C36 108.8(2) . . ?
C34 C35 C36 105.2(2) . . ?
C48 C35 C42 107.5(2) . . ?
C34 C35 C42 107.7(2) . . ?
C36 C35 C42 113.5(2) . . ?
C37 C36 C41 118.0(3) . . ?
C37 C36 C35 121.6(3) . . ?
C41 C36 C35 120.3(3) . . ?
C36 C37 C38 120.9(3) . . ?
C39 C38 C37 120.4(3) . . ?
C38 C39 C40 119.5(3) . . ?
C39 C40 C41 120.7(3) . . ?
C40 C41 C36 120.6(3) . . ?
C43 C42 C47 118.5(3) . . ?
C43 C42 C35 123.1(3) . . ?
C47 C42 C35 118.4(3) . . ?
C42 C43 C44 119.5(4) . . ?
C45 C44 C43 121.3(4) . . ?
C44 C45 C46 119.6(4) . . ?
C45 C46 C47 119.5(4) . . ?
C46 C47 C42 121.4(4) . . ?
N7 C48 C49 107.6(3) . . ?
N7 C48 C35 123.0(2) . . ?
C49 C48 C35 128.9(3) . . ?
C50 C49 C48 108.1(3) . . ?
C49 C50 C51 106.4(3) . . ?
N7 C51 C50 108.0(3) . . ?
N7 C51 C52 113.7(2) . . ?
C50 C51 C52 138.1(3) . . ?
N8 C52 C51 118.8(3) . . ?
C54 C53 C58 119.4(3) . . ?
C54 C53 N8 120.1(3) . . ?
C58 C53 N8 120.4(2) . . ?
C55 C54 C53 120.1(3) . . ?
C54 C55 C56 120.6(3) . . ?
C55 C56 C57 119.8(3) . . ?
C56 C57 C58 119.9(3) . . ?
C57 C58 C53 120.1(3) . . ?
C57 C58 N1 122.0(3) . . ?
C53 C58 N1 117.4(2) . . ?
O3S C2S C1S 110.8(9) . . ?
C4S O3S C2S 112.2(7) . . ?
O3S C4S C5S 114.1(9) . . ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.990

_refine_diff_density_max         0.92
_refine_diff_density_min         -0.94
_refine_diff_density_rms         0.10

#===END of CIF

data_PDIMPY
_database_code_CSD               216098

_refine_special_details          
;
Disordered atoms C6, C7, C8, C25, C26, C27 modelled isotropically using
two-site occupancy model(60:40) and with appropriate geometric restraints
applied. Solvent isotropically modelled with 0.25 occupancy.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H32 N8 Pd2, 0.25(C H4 O)'
_chemical_formula_sum            'C38.25 H33 N8 O0.25 Pd2'
_chemical_formula_weight         821.53

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'
Pd Pd -0.9988 1.0072 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4559(8)
_cell_length_b                   13.2076(11)
_cell_length_c                   14.3084(12)
_cell_angle_alpha                74.331(2)
_cell_angle_beta                 86.576(2)
_cell_angle_gamma                81.503(2)
_cell_volume                     1701.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4076
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.7

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             825
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_process_details   '(SHELXTL version 6.12; Bruker, 2001)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14533
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.077
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7481
_reflns_number_gt                4880
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  
'SHELXL-97; enCIFer (CCDC, 2003); PLATON (Spek, 2003)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.026P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   
'placed geometrically; solvent H atoms not located'
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7474
_refine_ls_number_parameters     435
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0704
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   0.86
_refine_ls_restrained_S_all      0.87
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002

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 0.35389(3) 0.57857(2) 0.14830(2) 0.03015(9) Uani 1 1 d . . .
Pd2 Pd 0.39667(3) 0.84988(2) 0.17016(2) 0.02858(8) Uani 1 1 d . . .
N1 N 0.2436(3) 0.6562(2) 0.0242(2) 0.0299(7) Uani 1 1 d . . .
N2 N 0.1729(3) 0.5242(2) 0.1821(2) 0.0351(8) Uani 1 1 d . A .
N3 N 0.4211(3) 0.4951(2) 0.2745(2) 0.0332(7) Uani 1 1 d . A .
N4 N 0.5618(3) 0.6135(2) 0.1366(2) 0.0284(7) Uani 1 1 d . A .
N5 N 0.2826(3) 0.8531(2) 0.0489(2) 0.0275(7) Uani 1 1 d . B .
N6 N 0.2059(3) 0.8962(2) 0.2136(2) 0.0294(7) Uani 1 1 d . B .
N7 N 0.4677(3) 0.8631(2) 0.2889(2) 0.0318(7) Uani 1 1 d . B .
N8 N 0.6120(3) 0.8108(2) 0.1479(2) 0.0281(7) Uani 1 1 d . . .
C1 C 0.1163(4) 0.6269(3) 0.0258(3) 0.0329(9) Uani 1 1 d . . .
H1A H 0.0547 0.6547 -0.0279 0.040 Uiso 1 1 calc R . .
C2 C 0.0743(4) 0.5530(3) 0.1100(3) 0.0320(9) Uani 1 1 d . . .
C3 C -0.0415(4) 0.4976(3) 0.1445(3) 0.0379(10) Uani 1 1 d . . .
H3A H -0.1263 0.5015 0.1105 0.046 Uiso 1 1 calc R . .
C4 C -0.0092(4) 0.4362(3) 0.2373(3) 0.0387(10) Uani 1 1 d . A .
H4A H -0.0681 0.3899 0.2789 0.046 Uiso 1 1 calc R . .
C5 C 0.1267(4) 0.4544(3) 0.2593(3) 0.0388(10) Uani 1 1 d D . .
C6 C 0.1992(7) 0.4324(8) 0.3547(5) 0.046(3) Uiso 0.40 1 d PD A 1
C7 C 0.1753(16) 0.3177(9) 0.4027(10) 0.093(5) Uiso 0.40 1 d PD A 1
H7A H 0.1067 0.3161 0.4570 0.139 Uiso 0.40 1 calc PR A 1
H7B H 0.2663 0.2755 0.4268 0.139 Uiso 0.40 1 calc PR A 1
H7C H 0.1376 0.2880 0.3550 0.139 Uiso 0.40 1 calc PR A 1
C8 C 0.1181(14) 0.4994(11) 0.4163(9) 0.083(4) Uiso 0.40 1 d PD A 1
H8A H 0.1288 0.5742 0.3874 0.124 Uiso 0.40 1 calc PR A 1
H8B H 0.1565 0.4767 0.4820 0.124 Uiso 0.40 1 calc PR A 1
H8C H 0.0166 0.4909 0.4195 0.124 Uiso 0.40 1 calc PR A 1
C6' C 0.2163(5) 0.3931(5) 0.3505(4) 0.0367(18) Uiso 0.60 1 d PD A 2
C7' C 0.2335(7) 0.2728(5) 0.3663(5) 0.0432(17) Uiso 0.60 1 d PD A 2
H7'A H 0.2908 0.2535 0.3127 0.065 Uiso 0.60 1 calc PR A 2
H7'B H 0.1391 0.2500 0.3685 0.065 Uiso 0.60 1 calc PR A 2
H7'C H 0.2818 0.2378 0.4277 0.065 Uiso 0.60 1 calc PR A 2
C8' C 0.1332(8) 0.4157(7) 0.4407(5) 0.065(2) Uiso 0.60 1 d PD A 2
H8'A H 0.1201 0.4921 0.4348 0.098 Uiso 0.60 1 calc PR A 2
H8'B H 0.1872 0.3780 0.4992 0.098 Uiso 0.60 1 calc PR A 2
H8'C H 0.0395 0.3912 0.4454 0.098 Uiso 0.60 1 calc PR A 2
C9 C 0.3614(4) 0.4321(3) 0.3504(3) 0.0404(10) Uani 1 1 d D . .
C10 C 0.4609(4) 0.3980(3) 0.4254(3) 0.0464(11) Uani 1 1 d . A .
H10A H 0.4469 0.3520 0.4879 0.056 Uiso 1 1 calc R . .
C11 C 0.5833(4) 0.4439(3) 0.3914(3) 0.0442(10) Uani 1 1 d . . .
H11A H 0.6687 0.4354 0.4261 0.053 Uiso 1 1 calc R A .
C12 C 0.5567(4) 0.5052(3) 0.2961(3) 0.0313(9) Uani 1 1 d . A .
C13 C 0.6269(4) 0.5710(3) 0.2198(3) 0.0317(9) Uani 1 1 d . . .
H13A H 0.7205 0.5848 0.2280 0.038 Uiso 1 1 calc R A .
C14 C 0.6355(3) 0.6785(3) 0.0589(3) 0.0271(8) Uani 1 1 d . . .
C15 C 0.6758(4) 0.6478(3) -0.0252(3) 0.0314(9) Uani 1 1 d . A .
H15A H 0.6494 0.5839 -0.0330 0.038 Uiso 1 1 calc R . .
C16 C 0.7538(4) 0.7088(3) -0.0978(3) 0.0389(10) Uani 1 1 d . . .
H16A H 0.7815 0.6865 -0.1548 0.047 Uiso 1 1 calc R A .
C17 C 0.7918(4) 0.8025(3) -0.0876(3) 0.0378(10) Uani 1 1 d . A .
H17A H 0.8476 0.8436 -0.1369 0.045 Uiso 1 1 calc R . .
C18 C 0.7485(4) 0.8363(3) -0.0059(3) 0.0343(9) Uani 1 1 d . . .
H18A H 0.7722 0.9017 0.0000 0.041 Uiso 1 1 calc R A .
C19 C 0.6707(3) 0.7754(3) 0.0675(3) 0.0273(8) Uani 1 1 d . A .
C20 C 0.6877(4) 0.8175(3) 0.2191(3) 0.0320(9) Uani 1 1 d . . .
H20A H 0.7890 0.8017 0.2181 0.038 Uiso 1 1 calc R . .
C21 C 0.6143(4) 0.8489(3) 0.2972(3) 0.0307(9) Uani 1 1 d . . .
C22 C 0.6449(4) 0.8693(3) 0.3847(3) 0.0397(10) Uani 1 1 d . . .
H22A H 0.7369 0.8659 0.4096 0.048 Uiso 1 1 calc R . .
C23 C 0.5146(4) 0.8954(3) 0.4274(3) 0.0432(10) Uani 1 1 d . B .
H23A H 0.5009 0.9124 0.4880 0.052 Uiso 1 1 calc R . .
C24 C 0.4057(4) 0.8926(3) 0.3659(3) 0.0375(9) Uani 1 1 d D . .
C25 C 0.2435(6) 0.9261(8) 0.3799(5) 0.037(4) Uiso 0.40 1 d PD B 1
C26 C 0.2105(13) 1.0329(8) 0.4061(9) 0.049(3) Uiso 0.40 1 d PD B 1
H26A H 0.2413 1.0894 0.3524 0.074 Uiso 0.40 1 calc PR B 1
H26B H 0.2618 1.0289 0.4648 0.074 Uiso 0.40 1 calc PR B 1
H26C H 0.1074 1.0484 0.4179 0.074 Uiso 0.40 1 calc PR B 1
C27 C 0.1925(11) 0.8389(8) 0.4657(7) 0.047(3) Uiso 0.40 1 d PD B 1
H27A H 0.1496 0.8710 0.5168 0.071 Uiso 0.40 1 calc PR B 1
H27B H 0.2744 0.7859 0.4917 0.071 Uiso 0.40 1 calc PR B 1
H27C H 0.1214 0.8045 0.4430 0.071 Uiso 0.40 1 calc PR B 1
C25' C 0.2443(5) 0.8985(6) 0.3840(4) 0.036(2) Uiso 0.60 1 d PD B 2
C26' C 0.2027(8) 0.9861(6) 0.4362(5) 0.051(2) Uiso 0.60 1 d PD B 2
H26D H 0.2230 1.0542 0.3933 0.077 Uiso 0.60 1 calc PR B 2
H26E H 0.2581 0.9696 0.4954 0.077 Uiso 0.60 1 calc PR B 2
H26F H 0.1005 0.9906 0.4531 0.077 Uiso 0.60 1 calc PR B 2
C27' C 0.2111(7) 0.7910(5) 0.4505(5) 0.0447(19) Uiso 0.60 1 d PD B 2
H27D H 0.2415 0.7349 0.4177 0.067 Uiso 0.60 1 calc PR B 2
H27E H 0.1081 0.7949 0.4647 0.067 Uiso 0.60 1 calc PR B 2
H27F H 0.2628 0.7751 0.5112 0.067 Uiso 0.60 1 calc PR B 2
C28 C 0.1564(4) 0.9273(3) 0.2922(3) 0.0358(9) Uani 1 1 d D . .
C29 C 0.0102(4) 0.9677(3) 0.2773(3) 0.0410(10) Uani 1 1 d . B .
H29A H -0.0528 0.9958 0.3212 0.049 Uiso 1 1 calc R . .
C30 C -0.0251(4) 0.9592(3) 0.1877(3) 0.0389(10) Uani 1 1 d . . .
H30A H -0.1163 0.9801 0.1587 0.047 Uiso 1 1 calc R B .
C31 C 0.1000(4) 0.9135(3) 0.1474(3) 0.0304(8) Uani 1 1 d . B .
C32 C 0.1464(4) 0.8859(3) 0.0614(3) 0.0303(9) Uani 1 1 d . . .
H32A H 0.0799 0.8908 0.0126 0.036 Uiso 1 1 calc R B .
C33 C 0.2971(4) 0.7313(3) -0.0556(3) 0.0297(8) Uani 1 1 d . B .
C34 C 0.3267(3) 0.8264(3) -0.0403(3) 0.0277(8) Uani 1 1 d . . .
C35 C 0.3979(4) 0.8939(3) -0.1129(3) 0.0344(9) Uani 1 1 d . B .
H35A H 0.4226 0.9569 -0.1021 0.041 Uiso 1 1 calc R . .
C36 C 0.4331(4) 0.8714(3) -0.2002(3) 0.0378(10) Uani 1 1 d . . .
H36A H 0.4808 0.9190 -0.2494 0.045 Uiso 1 1 calc R B .
C37 C 0.3991(4) 0.7794(3) -0.2164(3) 0.0407(10) Uani 1 1 d . B .
H37A H 0.4214 0.7646 -0.2774 0.049 Uiso 1 1 calc R . .
C38 C 0.3328(4) 0.7091(3) -0.1440(3) 0.0390(10) Uani 1 1 d . . .
H38A H 0.3115 0.6451 -0.1548 0.047 Uiso 1 1 calc R B .
C1S C -0.0761(16) 0.6342(12) 0.3154(11) 0.039(4) Uiso 0.25 1 d P . .
O1S O 0.049(2) 0.6817(16) 0.3317(14) 0.134(7) Uiso 0.25 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.02516(16) 0.03583(19) 0.03200(18) -0.01184(14) -0.00138(13) -0.00660(13)
Pd2 0.02253(15) 0.02906(17) 0.03475(18) -0.00892(13) -0.00468(13) -0.00293(12)
N1 0.0262(16) 0.0275(17) 0.0390(19) -0.0132(15) -0.0049(14) -0.0030(13)
N2 0.0249(16) 0.047(2) 0.0383(19) -0.0169(16) 0.0021(15) -0.0107(14)
N3 0.0304(17) 0.044(2) 0.0272(18) -0.0110(15) -0.0001(14) -0.0098(14)
N4 0.0220(15) 0.0268(17) 0.0367(18) -0.0090(14) -0.0019(14) -0.0031(13)
N5 0.0257(16) 0.0205(16) 0.0360(18) -0.0068(13) -0.0068(14) -0.0015(12)
N6 0.0203(15) 0.0330(18) 0.0329(18) -0.0055(14) 0.0008(13) -0.0036(13)
N7 0.0290(17) 0.0336(18) 0.0335(18) -0.0087(15) -0.0033(14) -0.0062(14)
N8 0.0244(15) 0.0221(16) 0.0387(18) -0.0096(14) -0.0035(14) -0.0021(12)
C1 0.030(2) 0.030(2) 0.043(2) -0.0167(19) -0.0085(18) 0.0023(17)
C2 0.0232(19) 0.031(2) 0.044(2) -0.0153(19) -0.0035(17) 0.0019(16)
C3 0.0231(19) 0.041(2) 0.055(3) -0.024(2) 0.0009(19) -0.0018(17)
C4 0.026(2) 0.052(3) 0.042(2) -0.017(2) 0.0100(18) -0.0127(18)
C5 0.030(2) 0.057(3) 0.035(2) -0.019(2) 0.0064(18) -0.0106(19)
C9 0.038(2) 0.059(3) 0.030(2) -0.018(2) 0.0032(18) -0.016(2)
C10 0.052(3) 0.059(3) 0.028(2) -0.004(2) -0.002(2) -0.019(2)
C11 0.040(2) 0.051(3) 0.041(3) -0.009(2) -0.008(2) -0.009(2)
C12 0.028(2) 0.034(2) 0.035(2) -0.0120(18) -0.0024(17) -0.0062(17)
C13 0.0211(19) 0.030(2) 0.046(2) -0.0149(19) -0.0054(18) 0.0015(16)
C14 0.0192(17) 0.0240(19) 0.035(2) -0.0049(17) -0.0042(16) 0.0028(15)
C15 0.031(2) 0.023(2) 0.039(2) -0.0096(17) -0.0042(18) 0.0053(16)
C16 0.031(2) 0.043(3) 0.034(2) -0.0055(19) -0.0003(18) 0.0111(19)
C17 0.026(2) 0.035(2) 0.044(3) 0.0006(19) -0.0006(18) 0.0009(17)
C18 0.028(2) 0.025(2) 0.047(2) -0.0021(18) -0.0040(18) -0.0055(16)
C19 0.0198(18) 0.027(2) 0.034(2) -0.0080(17) -0.0090(16) 0.0028(15)
C20 0.0243(19) 0.025(2) 0.044(2) -0.0027(18) -0.0080(18) -0.0047(16)
C21 0.029(2) 0.028(2) 0.032(2) -0.0027(17) -0.0084(17) -0.0025(16)
C22 0.037(2) 0.045(3) 0.034(2) -0.0005(19) -0.0128(19) -0.0101(19)
C23 0.048(3) 0.056(3) 0.027(2) -0.010(2) -0.0011(19) -0.011(2)
C24 0.036(2) 0.042(2) 0.031(2) -0.0032(19) -0.0019(18) -0.0075(18)
C28 0.030(2) 0.039(2) 0.036(2) -0.0043(19) 0.0033(18) -0.0094(17)
C29 0.026(2) 0.054(3) 0.040(2) -0.009(2) 0.0087(18) -0.0042(19)
C30 0.024(2) 0.039(2) 0.049(3) -0.001(2) 0.0012(18) -0.0082(17)
C31 0.0251(19) 0.027(2) 0.036(2) -0.0026(17) -0.0020(17) -0.0053(16)
C32 0.027(2) 0.021(2) 0.041(2) -0.0006(17) -0.0102(17) -0.0053(16)
C33 0.0269(19) 0.025(2) 0.037(2) -0.0081(17) -0.0091(17) 0.0009(15)
C34 0.0242(18) 0.024(2) 0.034(2) -0.0082(17) -0.0098(16) 0.0038(15)
C35 0.032(2) 0.024(2) 0.045(2) -0.0052(18) -0.0083(18) 0.0010(16)
C36 0.036(2) 0.035(2) 0.034(2) 0.0003(19) -0.0025(18) 0.0014(18)
C37 0.041(2) 0.047(3) 0.034(2) -0.012(2) -0.0052(19) -0.001(2)
C38 0.038(2) 0.039(2) 0.044(3) -0.016(2) -0.008(2) -0.0031(19)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N1 2.053(3) . ?
Pd1 N2 1.938(3) . ?
Pd1 N3 1.932(3) . ?
Pd1 N4 2.072(3) . ?
Pd2 N5 2.084(3) . ?
Pd2 N6 1.939(3) . ?
Pd2 N7 1.923(3) . ?
Pd2 N8 2.053(3) . ?
N1 C1 1.315(4) . ?
N1 C33 1.418(4) . ?
N2 C5 1.331(4) . ?
N2 C2 1.370(4) . ?
N3 C9 1.330(4) . ?
N3 C12 1.370(4) . ?
N4 C13 1.318(4) . ?
N4 C14 1.424(4) . ?
N5 C32 1.314(4) . ?
N5 C34 1.437(4) . ?
N6 C28 1.334(4) . ?
N6 C31 1.371(4) . ?
N7 C24 1.341(4) . ?
N7 C21 1.379(4) . ?
N8 C20 1.309(4) . ?
N8 C19 1.411(4) . ?
C1 C2 1.408(5) . ?
C2 C3 1.398(5) . ?
C3 C4 1.382(5) . ?
C4 C5 1.410(5) . ?
C5 C6 1.502(6) . ?
C5 C6' 1.560(5) . ?
C6 C8 1.514(7) . ?
C6 C7 1.528(8) . ?
C6 C9 1.531(6) . ?
C6' C7' 1.528(6) . ?
C6' C9 1.535(5) . ?
C6' C8' 1.547(6) . ?
C9 C10 1.405(5) . ?
C10 C11 1.387(5) . ?
C11 C12 1.402(5) . ?
C12 C13 1.399(5) . ?
C14 C15 1.386(5) . ?
C14 C19 1.407(5) . ?
C15 C16 1.380(5) . ?
C16 C17 1.384(5) . ?
C17 C18 1.380(5) . ?
C18 C19 1.385(5) . ?
C20 C21 1.405(5) . ?
C21 C22 1.405(5) . ?
C22 C23 1.381(5) . ?
C23 C24 1.404(5) . ?
C24 C25' 1.527(5) . ?
C24 C25 1.549(6) . ?
C25 C28 1.537(6) . ?
C25 C26 1.539(7) . ?
C25 C27 1.549(7) . ?
C25' C28 1.526(5) . ?
C25' C26' 1.533(6) . ?
C25' C27' 1.544(6) . ?
C28 C29 1.414(5) . ?
C29 C30 1.380(5) . ?
C30 C31 1.411(5) . ?
C31 C32 1.404(5) . ?
C33 C38 1.385(5) . ?
C33 C34 1.401(5) . ?
C34 C35 1.386(5) . ?
C35 C36 1.370(5) . ?
C36 C37 1.382(5) . ?
C37 C38 1.380(5) . ?
C1S O1S 1.48(2) . ?

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
N3 Pd1 N2 88.06(13) . . ?
N3 Pd1 N1 168.31(12) . . ?
N2 Pd1 N1 80.28(12) . . ?
N3 Pd1 N4 80.76(12) . . ?
N2 Pd1 N4 168.58(12) . . ?
N1 Pd1 N4 110.93(12) . . ?
N7 Pd2 N6 88.19(12) . . ?
N7 Pd2 N8 80.08(12) . . ?
N6 Pd2 N8 168.03(12) . . ?
N7 Pd2 N5 168.55(11) . . ?
N6 Pd2 N5 80.72(12) . . ?
N8 Pd2 N5 110.86(11) . . ?
C1 N1 C33 123.0(3) . . ?
C1 N1 Pd1 112.0(3) . . ?
C33 N1 Pd1 124.9(2) . . ?
C5 N2 C2 110.7(3) . . ?
C5 N2 Pd1 133.1(3) . . ?
C2 N2 Pd1 115.8(2) . . ?
C9 N3 C12 110.1(3) . . ?
C9 N3 Pd1 134.0(2) . . ?
C12 N3 Pd1 115.9(2) . . ?
C13 N4 C14 118.8(3) . . ?
C13 N4 Pd1 110.1(2) . . ?
C14 N4 Pd1 131.0(2) . . ?
C32 N5 C34 118.0(3) . . ?
C32 N5 Pd2 110.1(2) . . ?
C34 N5 Pd2 131.9(2) . . ?
C28 N6 C31 111.0(3) . . ?
C28 N6 Pd2 132.8(2) . . ?
C31 N6 Pd2 115.7(2) . . ?
C24 N7 C21 109.4(3) . . ?
C24 N7 Pd2 133.8(2) . . ?
C21 N7 Pd2 116.5(2) . . ?
C20 N8 C19 124.0(3) . . ?
C20 N8 Pd2 112.3(2) . . ?
C19 N8 Pd2 123.6(2) . . ?
N1 C1 C2 117.7(3) . . ?
N2 C2 C3 107.2(3) . . ?
N2 C2 C1 113.8(3) . . ?
C3 C2 C1 139.0(4) . . ?
C4 C3 C2 107.0(3) . . ?
C3 C4 C5 107.9(3) . . ?
N2 C5 C4 107.2(3) . . ?
N2 C5 C6 119.5(4) . . ?
C4 C5 C6 131.0(4) . . ?
N2 C5 C6' 125.6(3) . . ?
C4 C5 C6' 126.6(4) . . ?
C5 C6 C8 109.9(7) . . ?
C5 C6 C7 102.0(8) . . ?
C8 C6 C7 106.6(9) . . ?
C5 C6 C9 116.6(5) . . ?
C8 C6 C9 114.6(8) . . ?
C7 C6 C9 105.8(8) . . ?
C7' C6' C9 111.4(4) . . ?
C7' C6' C8' 106.0(5) . . ?
C9 C6' C8' 105.7(5) . . ?
C7' C6' C5 112.6(4) . . ?
C9 C6' C5 112.9(4) . . ?
C8' C6' C5 107.7(5) . . ?
N3 C9 C10 108.2(3) . . ?
N3 C9 C6 119.6(4) . . ?
C10 C9 C6 129.8(4) . . ?
N3 C9 C6' 125.2(4) . . ?
C10 C9 C6' 126.2(4) . . ?
C11 C10 C9 107.4(4) . . ?
C10 C11 C12 106.8(4) . . ?
N3 C12 C13 113.6(3) . . ?
N3 C12 C11 107.6(3) . . ?
C13 C12 C11 138.8(4) . . ?
N4 C13 C12 119.3(3) . . ?
C15 C14 C19 118.8(3) . . ?
C15 C14 N4 121.5(3) . . ?
C19 C14 N4 119.8(3) . . ?
C16 C15 C14 120.8(4) . . ?
C15 C16 C17 120.1(4) . . ?
C18 C17 C16 119.9(4) . . ?
C17 C18 C19 120.4(4) . . ?
C18 C19 C14 119.9(3) . . ?
C18 C19 N8 122.6(3) . . ?
C14 C19 N8 117.2(3) . . ?
N8 C20 C21 117.8(3) . . ?
N7 C21 C22 108.0(3) . . ?
N7 C21 C20 113.1(3) . . ?
C22 C21 C20 138.9(3) . . ?
C23 C22 C21 106.4(3) . . ?
C22 C23 C24 108.4(3) . . ?
N7 C24 C23 107.8(3) . . ?
N7 C24 C25' 121.1(4) . . ?
C23 C24 C25' 130.1(4) . . ?
N7 C24 C25 125.6(4) . . ?
C23 C24 C25 126.4(4) . . ?
C28 C25 C26 110.7(7) . . ?
C28 C25 C27 105.9(6) . . ?
C26 C25 C27 108.2(8) . . ?
C28 C25 C24 112.7(5) . . ?
C26 C25 C24 112.7(7) . . ?
C27 C25 C24 106.2(6) . . ?
C28 C25' C24 114.6(4) . . ?
C28 C25' C26' 107.9(5) . . ?
C24 C25' C26' 105.9(5) . . ?
C28 C25' C27' 109.7(5) . . ?
C24 C25' C27' 108.8(5) . . ?
C26' C25' C27' 109.9(5) . . ?
N6 C28 C29 107.2(3) . . ?
N6 C28 C25' 121.3(4) . . ?
C29 C28 C25' 130.4(4) . . ?
N6 C28 C25 126.7(4) . . ?
C29 C28 C25 126.0(4) . . ?
C30 C29 C28 108.0(3) . . ?
C29 C30 C31 107.0(3) . . ?
N6 C31 C32 113.8(3) . . ?
N6 C31 C30 106.8(3) . . ?
C32 C31 C30 139.3(3) . . ?
N5 C32 C31 119.4(3) . . ?
C38 C33 C34 119.8(4) . . ?
C38 C33 N1 122.0(3) . . ?
C34 C33 N1 117.9(3) . . ?
C35 C34 C33 118.7(3) . . ?
C35 C34 N5 121.0(3) . . ?
C33 C34 N5 120.2(3) . . ?
C36 C35 C34 121.1(4) . . ?
C35 C36 C37 120.0(4) . . ?
C38 C37 C36 120.0(4) . . ?
C37 C38 C33 120.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.955
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.955
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.53
_refine_diff_density_rms         0.09

#===END of CIF

data_pyrbzi
_database_code_CSD               216099

_refine_special_details          
;
Disorder present in all pTsO groups except that of S4. Those of S1 and S2
have all carbons except the C attached to S modelled over 2 sites, with
occupancies 0.5:0.5 and 0.6:0.4 respectively. That of S3 is half occupied
and has the sulfur and two of the three oxygens modelled over 2 0.25
occupied sites. There are also several partially occupied methanol molecules,
one half methanol required to be methoxide for charge neutrality. NH protons
could all be clearly located from difference Fourier syntheses.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C38H40N8(C7H7SO3)3.5(CH3O)0.5(CH4O)1.5
_chemical_formula_sum            'C64.50 H72 N8 O12.50 S3.50'
_chemical_formula_weight         1271.52

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.9007(10)
_cell_length_b                   16.2779(13)
_cell_length_c                   18.0091(14)
_cell_angle_alpha                75.638(1)
_cell_angle_beta                 75.199(1)
_cell_angle_gamma                85.938(1)
_cell_volume                     3542.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6260
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.9

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1343
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            32396
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         28.97
_reflns_number_total             16861
_reflns_number_gt                9650
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1703P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16844
_refine_ls_number_parameters     765
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0843
_refine_ls_wR_factor_ref         0.2704
_refine_ls_wR_factor_gt          0.2392
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
S1 S 0.33737(7) 0.26837(5) 0.25891(5) 0.0311(2) Uani 1 1 d . A .
S2 S 0.30247(7) 0.58053(5) 0.33415(5) 0.0330(2) Uani 1 1 d . B .
S4 S 0.21886(8) 0.08945(6) 0.59475(6) 0.0412(2) Uani 1 1 d . . .
O1 O 0.2626(2) 0.28373(17) 0.20934(15) 0.0433(6) Uani 1 1 d . . .
O2 O 0.28555(19) 0.23321(17) 0.34252(14) 0.0417(6) Uani 1 1 d . . .
O3 O 0.4029(2) 0.34190(16) 0.24938(15) 0.0424(6) Uani 1 1 d . . .
O4 O 0.1907(2) 0.60354(18) 0.35779(17) 0.0541(8) Uani 1 1 d . . .
O5 O 0.31482(18) 0.50482(14) 0.30118(13) 0.0315(5) Uani 1 1 d . . .
O6 O 0.3623(3) 0.5711(2) 0.39297(17) 0.0600(8) Uani 1 1 d . . .
O10 O 0.1422(3) 0.02074(19) 0.6171(2) 0.0778(11) Uani 1 1 d . . .
O11 O 0.23661(19) 0.12924(16) 0.51062(15) 0.0402(6) Uani 1 1 d . . .
O12 O 0.3183(3) 0.06658(19) 0.61802(18) 0.0611(8) Uani 1 1 d . . .
N1 N 0.4501(2) 0.17925(16) 0.44635(16) 0.0285(6) Uani 1 1 d . . .
H1A H 0.3798 0.1843 0.4563 0.034 Uiso 1 1 calc R . .
N2 N 0.5256(2) 0.40706(17) 0.33150(17) 0.0324(6) Uani 1 1 d . . .
H2A H 0.4785 0.3817 0.3172 0.039 Uiso 1 1 calc R . .
N3 N 0.5201(2) 0.49648(18) 0.16832(18) 0.0369(7) Uani 1 1 d . . .
H3A H 0.4811 0.4505 0.1899 0.044 Uiso 1 1 calc R . .
N4 N 0.3154(2) 0.51797(18) 0.14478(16) 0.0342(6) Uani 1 1 d . . .
H4A H 0.3217 0.5081 0.1937 0.041 Uiso 1 1 calc R . .
N5 N 0.1335(2) 0.44085(16) 0.27504(15) 0.0265(6) Uani 1 1 d . . .
H5A H 0.1841 0.4524 0.2957 0.032 Uiso 1 1 calc R . .
N6 N 0.0567(2) 0.22424(18) 0.40443(17) 0.0332(6) Uani 1 1 d . . .
H6A H 0.1251 0.2348 0.3824 0.040 Uiso 1 1 calc R . .
N7 N 0.1678(2) 0.06704(17) 0.37967(17) 0.0336(6) Uani 1 1 d . . .
H7A H 0.2064 0.1129 0.3686 0.040 Uiso 1 1 calc R . .
N8 N 0.3654(2) 0.03506(17) 0.40943(17) 0.0333(6) Uani 1 1 d . . .
H8A H 0.3197 0.0703 0.4310 0.040 Uiso 1 1 calc R . .
C1 C 0.5088(3) 0.1099(2) 0.4257(2) 0.0306(7) Uani 1 1 d . . .
C2 C 0.6174(3) 0.1277(2) 0.4144(2) 0.0376(8) Uani 1 1 d . . .
H2B H 0.6765 0.0918 0.3997 0.045 Uiso 1 1 calc R . .
C3 C 0.6224(3) 0.2064(2) 0.4284(2) 0.0391(8) Uani 1 1 d . . .
H3B H 0.6859 0.2349 0.4248 0.047 Uiso 1 1 calc R . .
C4 C 0.5169(3) 0.2374(2) 0.4489(2) 0.0295(7) Uani 1 1 d . . .
C5 C 0.4789(3) 0.3209(2) 0.4697(2) 0.0301(7) Uani 1 1 d . . .
C6 C 0.5021(3) 0.3203(2) 0.5502(2) 0.0420(9) Uani 1 1 d . . .
H6B H 0.5788 0.3104 0.5467 0.063 Uiso 1 1 calc R . .
H6C H 0.4609 0.2751 0.5916 0.063 Uiso 1 1 calc R . .
H6D H 0.4812 0.3751 0.5632 0.063 Uiso 1 1 calc R . .
C7 C 0.3582(3) 0.3363(2) 0.4753(2) 0.0319(7) Uani 1 1 d . . .
H7B H 0.3435 0.3363 0.4245 0.048 Uiso 1 1 calc R . .
H7C H 0.3372 0.3912 0.4880 0.048 Uiso 1 1 calc R . .
H7D H 0.3172 0.2911 0.5168 0.048 Uiso 1 1 calc R . .
C8 C 0.5425(3) 0.3896(2) 0.4046(2) 0.0324(7) Uani 1 1 d . . .
C9 C 0.6247(3) 0.4423(2) 0.4044(3) 0.0428(9) Uani 1 1 d . . .
H9A H 0.6527 0.4435 0.4481 0.051 Uiso 1 1 calc R . .
C10 C 0.6567(3) 0.4920(2) 0.3283(3) 0.0488(10) Uani 1 1 d . . .
H10A H 0.7118 0.5333 0.3102 0.059 Uiso 1 1 calc R . .
C11 C 0.5939(3) 0.4712(2) 0.2820(2) 0.0392(8) Uani 1 1 d . . .
C12 C 0.5887(3) 0.5129(2) 0.2055(2) 0.0392(8) Uani 1 1 d . . .
H12A H 0.6389 0.5569 0.1779 0.047 Uiso 1 1 calc R . .
C13 C 0.5047(3) 0.5481(2) 0.0954(2) 0.0371(8) Uani 1 1 d . . .
C14 C 0.5918(4) 0.5909(3) 0.0375(2) 0.0499(10) Uani 1 1 d . . .
H14A H 0.6620 0.5847 0.0460 0.060 Uiso 1 1 calc R . .
C15 C 0.5740(4) 0.6414(3) -0.0310(2) 0.0557(12) Uani 1 1 d . . .
H15A H 0.6325 0.6699 -0.0705 0.067 Uiso 1 1 calc R . .
C16 C 0.4723(4) 0.6517(3) -0.0437(2) 0.0592(13) Uani 1 1 d . . .
H16A H 0.4620 0.6869 -0.0920 0.071 Uiso 1 1 calc R . .
C17 C 0.3845(4) 0.6111(3) 0.0133(2) 0.0489(10) Uani 1 1 d . . .
H17A H 0.3144 0.6187 0.0047 0.059 Uiso 1 1 calc R . .
C18 C 0.4026(3) 0.5586(2) 0.0839(2) 0.0370(8) Uani 1 1 d . . .
C19 C 0.2254(3) 0.4938(2) 0.1344(2) 0.0348(8) Uani 1 1 d . . .
H19A H 0.2197 0.5012 0.0816 0.042 Uiso 1 1 calc R . .
C20 C 0.1394(3) 0.4586(2) 0.19435(19) 0.0305(7) Uani 1 1 d . . .
C21 C 0.0427(3) 0.4297(2) 0.1870(2) 0.0401(8) Uani 1 1 d . . .
H21A H 0.0231 0.4330 0.1389 0.048 Uiso 1 1 calc R . .
C22 C -0.0184(3) 0.3957(2) 0.2623(2) 0.0372(8) Uani 1 1 d . . .
H22A H -0.0874 0.3712 0.2753 0.045 Uiso 1 1 calc R . .
C23 C 0.0403(3) 0.4038(2) 0.31685(19) 0.0277(7) Uani 1 1 d . . .
C24 C 0.0085(3) 0.3755(2) 0.40585(19) 0.0300(7) Uani 1 1 d . . .
C25 C 0.0992(3) 0.3891(2) 0.4429(2) 0.0379(8) Uani 1 1 d . . .
H25A H 0.1626 0.3562 0.4236 0.057 Uiso 1 1 calc R . .
H25B H 0.0756 0.3702 0.5006 0.057 Uiso 1 1 calc R . .
H25C H 0.1172 0.4494 0.4280 0.057 Uiso 1 1 calc R . .
C26 C -0.0910(3) 0.4277(3) 0.4365(2) 0.0430(9) Uani 1 1 d . . .
H26A H -0.1489 0.4196 0.4129 0.065 Uiso 1 1 calc R . .
H26B H -0.0725 0.4880 0.4218 0.065 Uiso 1 1 calc R . .
H26C H -0.1146 0.4088 0.4942 0.065 Uiso 1 1 calc R . .
C27 C -0.0185(3) 0.2831(2) 0.4256(2) 0.0312(7) Uani 1 1 d . . .
C28 C -0.1157(3) 0.2416(2) 0.4598(2) 0.0409(9) Uani 1 1 d . . .
H28A H -0.1818 0.2668 0.4811 0.049 Uiso 1 1 calc R . .
C29 C -0.0990(3) 0.1557(2) 0.4575(2) 0.0452(9) Uani 1 1 d . . .
H29A H -0.1518 0.1126 0.4762 0.054 Uiso 1 1 calc R . .
C30 C 0.0097(3) 0.1457(2) 0.4227(2) 0.0368(8) Uani 1 1 d . . .
C31 C 0.0641(3) 0.0721(2) 0.4079(2) 0.0391(8) Uani 1 1 d . . .
H31A H 0.0231 0.0223 0.4191 0.047 Uiso 1 1 calc R . .
C32 C 0.2204(3) -0.0091(2) 0.3662(2) 0.0336(7) Uani 1 1 d . . .
C33 C 0.1752(3) -0.0661(2) 0.3363(2) 0.0470(10) Uani 1 1 d . . .
H33A H 0.1067 -0.0549 0.3252 0.056 Uiso 1 1 calc R . .
C34 C 0.2316(4) -0.1389(3) 0.3231(3) 0.0539(11) Uani 1 1 d . . .
H34A H 0.2019 -0.1774 0.3023 0.065 Uiso 1 1 calc R . .
C35 C 0.3304(4) -0.1561(2) 0.3398(3) 0.0500(10) Uani 1 1 d . . .
H35A H 0.3669 -0.2071 0.3317 0.060 Uiso 1 1 calc R . .
C36 C 0.3779(3) -0.0998(2) 0.3685(2) 0.0404(8) Uani 1 1 d . . .
H36A H 0.4466 -0.1116 0.3790 0.048 Uiso 1 1 calc R . .
C37 C 0.3224(3) -0.0266(2) 0.3812(2) 0.0326(7) Uani 1 1 d . . .
C38 C 0.4666(3) 0.0435(2) 0.40592(19) 0.0296(7) Uani 1 1 d . . .
H38A H 0.5152 0.0015 0.3887 0.036 Uiso 1 1 calc R . .
C39 C 0.4282(3) 0.1888(2) 0.2294(2) 0.0391(8) Uiso 1 1 d . . .
C40A C 0.3748(9) 0.1260(6) 0.2026(6) 0.044(2) Uiso 0.50 1 d P A 1
H40A H 0.3032 0.1334 0.1971 0.052 Uiso 0.50 1 calc PR A 1
C41A C 0.4379(8) 0.0558(6) 0.1863(5) 0.047(2) Uiso 0.50 1 d P A 1
H41A H 0.4081 0.0124 0.1715 0.056 Uiso 0.50 1 calc PR A 1
C42A C 0.5459(9) 0.0494(5) 0.1917(5) 0.0404(18) Uiso 0.50 1 d P A 1
C43A C 0.5895(7) 0.1100(6) 0.2139(5) 0.0407(19) Uiso 0.50 1 d P A 1
H43A H 0.6621 0.1070 0.2171 0.049 Uiso 0.50 1 calc PR A 1
C44A C 0.5216(8) 0.1779(6) 0.2319(6) 0.045(3) Uiso 0.50 1 d P A 1
H44A H 0.5523 0.2200 0.2479 0.054 Uiso 0.50 1 calc PR A 1
C45A C 0.6131(9) -0.0310(7) 0.1744(7) 0.071(3) Uiso 0.50 1 d P A 1
H45A H 0.6856 -0.0269 0.1808 0.106 Uiso 0.50 1 calc PR A 1
H45B H 0.6171 -0.0343 0.1201 0.106 Uiso 0.50 1 calc PR A 1
H45C H 0.5785 -0.0821 0.2115 0.106 Uiso 0.50 1 calc PR A 1
C40B C 0.4062(9) 0.1259(6) 0.2067(6) 0.045(3) Uiso 0.50 1 d P A 2
H40C H 0.3350 0.1205 0.2030 0.054 Uiso 0.50 1 calc PR A 2
C41B C 0.4852(11) 0.0613(6) 0.1858(6) 0.053(2) Uiso 0.50 1 d P A 2
H41B H 0.4665 0.0149 0.1687 0.064 Uiso 0.50 1 calc PR A 2
C42B C 0.5873(9) 0.0700(7) 0.1919(6) 0.053(2) Uiso 0.50 1 d P A 2
C43B C 0.6171(9) 0.1354(6) 0.2167(6) 0.053(2) Uiso 0.50 1 d P A 2
H43B H 0.6887 0.1390 0.2204 0.063 Uiso 0.50 1 calc PR A 2
C44B C 0.5425(7) 0.1959(6) 0.2363(5) 0.035(2) Uiso 0.50 1 d P A 2
H44B H 0.5619 0.2417 0.2540 0.042 Uiso 0.50 1 calc PR A 2
C45B C 0.6658(10) -0.0022(8) 0.1724(8) 0.082(3) Uiso 0.50 1 d P A 2
H45D H 0.7366 0.0093 0.1779 0.123 Uiso 0.50 1 calc PR A 2
H45E H 0.6713 -0.0057 0.1180 0.123 Uiso 0.50 1 calc PR A 2
H45F H 0.6392 -0.0561 0.2089 0.123 Uiso 0.50 1 calc PR A 2
C46 C 0.3634(3) 0.6623(2) 0.2524(2) 0.0423(9) Uiso 1 1 d . . .
C47A C 0.3183(7) 0.7032(5) 0.1976(5) 0.042(2) Uiso 0.60 1 d P B 1
H47A H 0.2456 0.6910 0.2025 0.051 Uiso 0.60 1 calc PR B 1
C48A C 0.3708(10) 0.7651(6) 0.1309(5) 0.054(2) Uiso 0.60 1 d P B 1
H48A H 0.3326 0.7948 0.0936 0.065 Uiso 0.60 1 calc PR B 1
C49A C 0.4740(8) 0.7816(5) 0.1205(5) 0.0461(18) Uiso 0.60 1 d P B 1
C50A C 0.5294(7) 0.7381(5) 0.1779(5) 0.0462(18) Uiso 0.60 1 d P B 1
H50A H 0.6028 0.7504 0.1704 0.055 Uiso 0.60 1 calc PR B 1
C51A C 0.4798(6) 0.6791(5) 0.2436(4) 0.0345(16) Uiso 0.60 1 d P B 1
H51A H 0.5169 0.6501 0.2818 0.041 Uiso 0.60 1 calc PR B 1
C52A C 0.5327(9) 0.8448(7) 0.0467(7) 0.083(3) Uiso 0.60 1 d P B 1
H52A H 0.4827 0.8690 0.0140 0.125 Uiso 0.60 1 calc PR B 1
H52B H 0.5915 0.8159 0.0164 0.125 Uiso 0.60 1 calc PR B 1
H52C H 0.5618 0.8904 0.0620 0.125 Uiso 0.60 1 calc PR B 1
C47B C 0.2814(11) 0.7036(7) 0.2028(7) 0.040(3) Uiso 0.40 1 d P B 2
H47B H 0.2077 0.6889 0.2177 0.047 Uiso 0.40 1 calc PR B 2
C48B C 0.3275(12) 0.7640(8) 0.1346(8) 0.054(4) Uiso 0.40 1 d P B 2
H48B H 0.2829 0.7911 0.1010 0.065 Uiso 0.40 1 calc PR B 2
C49B C 0.4311(15) 0.7862(8) 0.1133(8) 0.054(3) Uiso 0.40 1 d P B 2
C50B C 0.4982(11) 0.7532(9) 0.1571(9) 0.053(3) Uiso 0.40 1 d P B 2
H50B H 0.5712 0.7697 0.1426 0.064 Uiso 0.40 1 calc PR B 2
C51B C 0.4524(10) 0.6881(8) 0.2309(7) 0.045(3) Uiso 0.40 1 d P B 2
H51C H 0.4992 0.6651 0.2640 0.054 Uiso 0.40 1 calc PR B 2
C52B C 0.4839(14) 0.8523(11) 0.0355(10) 0.085(5) Uiso 0.40 1 d P B 2
H52D H 0.5599 0.8583 0.0330 0.127 Uiso 0.40 1 calc PR B 2
H52E H 0.4475 0.9073 0.0353 0.127 Uiso 0.40 1 calc PR B 2
H52F H 0.4775 0.8328 -0.0104 0.127 Uiso 0.40 1 calc PR B 2
C60 C 0.1598(3) 0.1698(2) 0.6431(2) 0.0344(8) Uiso 1 1 d . . .
C61 C 0.0637(3) 0.2055(2) 0.6297(2) 0.0389(8) Uiso 1 1 d . . .
H61A H 0.0293 0.1859 0.5966 0.047 Uiso 1 1 calc R . .
C62 C 0.0183(3) 0.2700(3) 0.6652(2) 0.0445(9) Uiso 1 1 d . . .
H62A H -0.0479 0.2942 0.6563 0.053 Uiso 1 1 calc R . .
C63 C 0.0665(3) 0.3001(3) 0.7131(2) 0.0467(9) Uiso 1 1 d . . .
C64 C 0.1633(3) 0.2656(3) 0.7247(3) 0.0503(10) Uiso 1 1 d . . .
H64A H 0.1983 0.2867 0.7565 0.060 Uiso 1 1 calc R . .
C65 C 0.2107(3) 0.1997(3) 0.6898(2) 0.0465(9) Uiso 1 1 d . . .
H65A H 0.2773 0.1759 0.6982 0.056 Uiso 1 1 calc R . .
C66 C 0.0147(4) 0.3708(3) 0.7527(3) 0.0715(14) Uiso 1 1 d . . .
H66A H 0.0603 0.3836 0.7843 0.107 Uiso 1 1 calc R . .
H66B H -0.0559 0.3524 0.7872 0.107 Uiso 1 1 calc R . .
H66C H 0.0063 0.4217 0.7121 0.107 Uiso 1 1 calc R . .
O1M O 0.1551(6) 0.5825(5) 0.9560(5) 0.084(2) Uiso 0.50 1 d PD C 1
C1M C 0.1978(8) 0.6243(6) 0.8784(5) 0.063(2) Uiso 0.50 1 d PD C 1
C1M" C 0.289(2) 0.6555(16) 0.8520(15) 0.088(7) Uiso 0.25 1 d PD D 3
O1M" O 0.234(2) 0.6968(18) 0.7976(16) 0.176(10) Uiso 0.25 1 d PD D 3
O2M O -0.1613(11) 0.1912(9) 1.0230(8) 0.169(5) Uiso 0.50 1 d PD . .
C2M C -0.1368(15) 0.2492(11) 0.9516(10) 0.137(6) Uiso 0.50 1 d PD . .
C3M C -0.0540(10) 0.1641(7) 1.2427(8) 0.089(4) Uiso 0.50 1 d PD . .
O3M O -0.0151(12) 0.0819(8) 1.2629(9) 0.082(4) Uiso 0.25 1 d PD E 1
O3M' O -0.1122(11) 0.1017(8) 1.2343(8) 0.070(4) Uiso 0.25 1 d PD E 2
O4M O -0.018(3) 0.074(2) 0.849(2) 0.212(14) Uiso 0.25 1 d PD . .
C4M C 0.041(3) 0.005(2) 0.878(2) 0.130(11) Uiso 0.25 1 d PD . .
S3 S 0.1211(4) 0.3713(6) 0.9462(4) 0.050(3) Uani 0.25 1 d PD F 1
O10' O 0.1913(6) 0.3900(5) 0.8652(4) 0.0156(16) Uiso 0.25 1 d PD F 1
O10" O 0.1422(13) 0.4145(10) 0.9952(8) 0.049(4) Uiso 0.25 1 d PD F 1
O101 O 0.1428(16) 0.4365(10) 0.9848(11) 0.068(6) Uiso 0.25 1 d PD F 2
O103 O 0.2165(6) 0.3550(6) 0.8726(5) 0.0215(18) Uiso 0.25 1 d PD F 2
S3' S 0.1249(4) 0.3705(6) 0.9363(5) 0.064(4) Uani 0.25 1 d PD F 2
O102 O 0.0084(4) 0.3740(4) 0.9418(4) 0.0668(17) Uiso 0.50 1 d PD . .
C101 C 0.1464(7) 0.2644(6) 0.9913(6) 0.057(2) Uiso 0.50 1 d PD . .
C102 C 0.1572(7) 0.2453(6) 1.0687(6) 0.060(2) Uiso 0.50 1 d P F .
H10B H 0.1521 0.2886 1.0965 0.072 Uiso 0.50 1 calc PR . .
C106 C 0.1609(9) 0.1984(8) 0.9526(7) 0.080(3) Uiso 0.50 1 d P F .
H10C H 0.1658 0.2126 0.8973 0.095 Uiso 0.50 1 calc PR . .
C103 C 0.1741(10) 0.1681(8) 1.1015(8) 0.089(4) Uiso 0.50 1 d P . .
H10D H 0.1794 0.1568 1.1548 0.107 Uiso 0.50 1 calc PR F .
C105 C 0.1680(12) 0.1202(10) 0.9866(9) 0.112(5) Uiso 0.50 1 d P . .
H10E H 0.1616 0.0775 0.9605 0.134 Uiso 0.50 1 calc PR F .
C104 C 0.1861(12) 0.0969(8) 1.0664(9) 0.107(4) Uiso 0.50 1 d PD F .
C107 C 0.2175(14) 0.0064(9) 1.1034(10) 0.126(5) Uiso 0.50 1 d PD . .
H10F H 0.2194 0.0021 1.1583 0.189 Uiso 0.50 1 calc PR F .
H10G H 0.2885 -0.0074 1.0733 0.189 Uiso 0.50 1 calc PR . .
H10H H 0.1648 -0.0334 1.1022 0.189 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0319(4) 0.0321(4) 0.0275(4) -0.0074(3) -0.0044(3) 0.0020(3)
S2 0.0396(5) 0.0324(4) 0.0302(4) -0.0131(3) -0.0082(4) -0.0019(3)
S4 0.0441(5) 0.0278(4) 0.0471(6) -0.0136(4) -0.0002(4) 0.0060(4)
O1 0.0458(15) 0.0491(16) 0.0386(15) -0.0120(12) -0.0169(12) 0.0047(12)
O2 0.0338(13) 0.0582(17) 0.0289(13) -0.0082(12) -0.0047(10) 0.0080(12)
O3 0.0473(15) 0.0354(14) 0.0468(15) -0.0139(12) -0.0107(12) -0.0027(11)
O4 0.0539(17) 0.0503(17) 0.0488(17) -0.0132(14) 0.0009(14) 0.0151(13)
O5 0.0310(12) 0.0318(12) 0.0331(13) -0.0121(10) -0.0053(10) -0.0024(9)
O6 0.081(2) 0.0623(19) 0.0489(17) -0.0103(14) -0.0335(16) -0.0242(17)
O10 0.079(2) 0.0355(16) 0.101(3) -0.0219(17) 0.019(2) -0.0132(15)
O11 0.0359(14) 0.0455(15) 0.0422(15) -0.0222(12) -0.0039(11) 0.0013(11)
O12 0.070(2) 0.0589(19) 0.0546(18) -0.0191(15) -0.0190(16) 0.0333(16)
N1 0.0253(13) 0.0257(13) 0.0361(15) -0.0107(11) -0.0071(11) 0.0003(10)
N2 0.0286(15) 0.0278(14) 0.0414(17) -0.0064(12) -0.0102(12) -0.0036(11)
N3 0.0336(16) 0.0303(15) 0.0389(17) -0.0061(13) 0.0043(13) -0.0044(12)
N4 0.0453(17) 0.0320(15) 0.0242(14) -0.0074(12) -0.0056(12) -0.0010(13)
N5 0.0276(14) 0.0285(14) 0.0263(14) -0.0095(11) -0.0093(11) 0.0021(11)
N6 0.0245(14) 0.0379(16) 0.0352(16) -0.0041(13) -0.0071(12) -0.0046(12)
N7 0.0349(16) 0.0265(14) 0.0409(17) -0.0073(12) -0.0112(13) -0.0044(12)
N8 0.0332(16) 0.0235(14) 0.0441(17) -0.0142(12) -0.0050(13) 0.0001(11)
C1 0.0338(18) 0.0249(16) 0.0320(17) -0.0066(13) -0.0074(14) 0.0036(13)
C2 0.0331(19) 0.0309(18) 0.050(2) -0.0103(16) -0.0137(16) 0.0069(14)
C3 0.0289(18) 0.0347(19) 0.058(2) -0.0121(17) -0.0186(17) 0.0017(14)
C4 0.0279(16) 0.0266(16) 0.0368(18) -0.0061(13) -0.0145(14) 0.0009(13)
C5 0.0320(17) 0.0265(16) 0.0373(18) -0.0097(14) -0.0166(14) 0.0009(13)
C6 0.051(2) 0.038(2) 0.045(2) -0.0126(17) -0.0240(18) -0.0004(17)
C7 0.0279(17) 0.0298(17) 0.0393(19) -0.0095(14) -0.0095(14) 0.0002(13)
C8 0.0282(17) 0.0256(16) 0.047(2) -0.0093(15) -0.0161(15) 0.0032(13)
C9 0.035(2) 0.0356(19) 0.063(3) -0.0073(18) -0.0237(18) -0.0038(15)
C10 0.031(2) 0.036(2) 0.079(3) -0.005(2) -0.019(2) -0.0085(16)
C11 0.0273(18) 0.0335(19) 0.053(2) -0.0062(16) -0.0060(16) -0.0031(14)
C12 0.0298(18) 0.0319(18) 0.049(2) -0.0104(16) 0.0042(16) -0.0034(14)
C13 0.047(2) 0.0269(17) 0.0308(18) -0.0090(14) 0.0046(15) -0.0054(15)
C14 0.056(3) 0.045(2) 0.040(2) -0.0137(18) 0.0115(19) -0.0135(19)
C15 0.074(3) 0.047(2) 0.035(2) -0.0083(18) 0.012(2) -0.023(2)
C16 0.093(4) 0.050(3) 0.028(2) -0.0047(18) -0.002(2) -0.017(2)
C17 0.070(3) 0.042(2) 0.032(2) -0.0052(16) -0.0085(19) -0.007(2)
C18 0.051(2) 0.0301(18) 0.0247(17) -0.0080(14) 0.0027(15) -0.0057(15)
C19 0.046(2) 0.0323(18) 0.0264(17) -0.0080(14) -0.0091(15) 0.0042(15)
C20 0.0337(18) 0.0308(17) 0.0297(17) -0.0095(13) -0.0117(14) 0.0037(13)
C21 0.049(2) 0.043(2) 0.035(2) -0.0118(16) -0.0210(17) 0.0056(17)
C22 0.0328(18) 0.042(2) 0.041(2) -0.0119(16) -0.0139(16) -0.0039(15)
C23 0.0268(16) 0.0263(16) 0.0328(17) -0.0105(13) -0.0094(13) 0.0023(12)
C24 0.0250(16) 0.0355(18) 0.0300(17) -0.0091(14) -0.0055(13) -0.0035(13)
C25 0.039(2) 0.048(2) 0.0289(18) -0.0078(15) -0.0094(15) -0.0127(16)
C26 0.036(2) 0.046(2) 0.045(2) -0.0162(18) -0.0023(17) 0.0033(16)
C27 0.0241(16) 0.0379(18) 0.0319(18) -0.0064(14) -0.0089(13) -0.0011(13)
C28 0.0247(17) 0.044(2) 0.051(2) -0.0059(17) -0.0064(16) -0.0041(15)
C29 0.0280(19) 0.041(2) 0.059(3) -0.0002(18) -0.0072(17) -0.0088(15)
C30 0.0269(17) 0.0335(18) 0.045(2) 0.0005(15) -0.0077(15) -0.0065(14)
C31 0.0327(19) 0.0345(19) 0.047(2) -0.0004(16) -0.0107(16) -0.0092(15)
C32 0.0379(19) 0.0283(17) 0.0343(18) -0.0086(14) -0.0076(15) 0.0001(14)
C33 0.053(2) 0.040(2) 0.055(2) -0.0135(18) -0.021(2) -0.0030(18)
C34 0.069(3) 0.040(2) 0.065(3) -0.022(2) -0.028(2) -0.004(2)
C35 0.068(3) 0.031(2) 0.058(3) -0.0230(18) -0.019(2) 0.0061(18)
C36 0.047(2) 0.0299(18) 0.048(2) -0.0151(16) -0.0138(18) 0.0030(15)
C37 0.0419(19) 0.0235(16) 0.0339(18) -0.0094(13) -0.0092(15) -0.0016(14)
C38 0.0346(18) 0.0234(15) 0.0272(16) -0.0045(13) -0.0032(14) 0.0013(13)
S3 0.021(4) 0.111(8) 0.010(2) -0.003(3) 0.006(2) -0.023(4)
S3' 0.068(7) 0.072(6) 0.066(6) -0.016(4) -0.039(5) -0.014(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
S1 O1 1.444(3) . ?
S1 O3 1.465(3) . ?
S1 O2 1.468(3) . ?
S1 C39 1.773(4) . ?
S2 O6 1.436(3) . ?
S2 O4 1.445(3) . ?
S2 O5 1.478(2) . ?
S2 C46 1.773(4) . ?
S4 O12 1.445(3) . ?
S4 O10 1.456(3) . ?
S4 O11 1.458(3) . ?
S4 C60 1.770(4) . ?
N1 C4 1.342(4) . ?
N1 C1 1.389(4) . ?
N2 C8 1.346(4) . ?
N2 C11 1.389(4) . ?
N3 C12 1.314(5) . ?
N3 C13 1.426(5) . ?
N4 C19 1.322(4) . ?
N4 C18 1.421(4) . ?
N5 C23 1.338(4) . ?
N5 C20 1.393(4) . ?
N6 C27 1.365(4) . ?
N6 C30 1.382(4) . ?
N7 C31 1.309(5) . ?
N7 C32 1.415(4) . ?
N8 C38 1.306(4) . ?
N8 C37 1.432(4) . ?
C1 C38 1.403(4) . ?
C1 C2 1.403(5) . ?
C2 C3 1.376(5) . ?
C3 C4 1.408(5) . ?
C4 C5 1.515(5) . ?
C5 C8 1.512(5) . ?
C5 C7 1.540(4) . ?
C5 C6 1.551(5) . ?
C8 C9 1.410(5) . ?
C9 C10 1.382(6) . ?
C10 C11 1.410(5) . ?
C11 C12 1.394(5) . ?
C13 C18 1.377(5) . ?
C13 C14 1.410(5) . ?
C14 C15 1.366(6) . ?
C15 C16 1.380(7) . ?
C16 C17 1.397(6) . ?
C17 C18 1.410(5) . ?
C19 C20 1.377(5) . ?
C20 C21 1.412(5) . ?
C21 C22 1.382(5) . ?
C22 C23 1.419(4) . ?
C23 C24 1.508(4) . ?
C24 C27 1.502(5) . ?
C24 C25 1.540(4) . ?
C24 C26 1.546(5) . ?
C27 C28 1.388(5) . ?
C28 C29 1.409(5) . ?
C29 C30 1.399(5) . ?
C30 C31 1.393(5) . ?
C32 C37 1.406(5) . ?
C32 C33 1.406(5) . ?
C33 C34 1.386(6) . ?
C34 C35 1.377(6) . ?
C35 C36 1.399(5) . ?
C36 C37 1.384(5) . ?
C39 C44A 1.216(10) . ?
C39 C40B 1.266(11) . ?
C39 C40A 1.506(11) . ?
C39 C44B 1.527(10) . ?
C40A C41A 1.403(14) . ?
C41A C42A 1.415(13) . ?
C42A C43A 1.356(13) . ?
C42A C45A 1.570(14) . ?
C43A C44A 1.410(14) . ?
C40B C41B 1.461(15) . ?
C41B C42B 1.369(15) . ?
C42B C43B 1.364(15) . ?
C42B C45B 1.545(16) . ?
C43B C44B 1.373(13) . ?
C46 C51B 1.185(13) . ?
C46 C47A 1.290(9) . ?
C46 C51A 1.507(8) . ?
C46 C47B 1.566(13) . ?
C47A C48A 1.413(12) . ?
C48A C49A 1.335(13) . ?
C49A C50A 1.423(12) . ?
C49A C52A 1.522(13) . ?
C50A C51A 1.366(10) . ?
C47B C48B 1.393(17) . ?
C48B C49B 1.34(2) . ?
C49B C50B 1.32(2) . ?
C49B C52B 1.57(2) . ?
C50B C51B 1.492(19) . ?
C60 C65 1.382(5) . ?
C60 C61 1.383(5) . ?
C61 C62 1.381(5) . ?
C62 C63 1.379(5) . ?
C63 C64 1.376(6) . ?
C63 C66 1.528(6) . ?
C64 C65 1.401(6) . ?
O1M C1M 1.381(9) . ?
C1M" O1M" 1.374(11) . ?
O2M C2M 1.369(10) . ?
C3M O3M' 1.363(10) . ?
C3M O3M 1.389(10) . ?
O4M C4M 1.369(11) . ?
S3 O10" 1.344(17) . ?
S3 O102 1.473(7) . ?
S3 O10' 1.479(6) . ?
S3 C101 1.774(13) . ?
O101 S3' 1.604(18) . ?
O103 S3' 1.478(7) . ?
S3' O102 1.479(7) . ?
S3' C101 1.807(13) . ?
C101 C102 1.391(13) . ?
C101 C106 1.397(14) . ?
C102 C103 1.278(15) . ?
C106 C105 1.276(18) . ?
C103 C104 1.434(18) . ?
C105 C104 1.47(2) . ?
C104 C107 1.531(9) . ?

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
O1 S1 O3 113.90(16) . . ?
O1 S1 O2 112.57(15) . . ?
O3 S1 O2 111.09(16) . . ?
O1 S1 C39 107.12(17) . . ?
O3 S1 C39 106.00(16) . . ?
O2 S1 C39 105.49(16) . . ?
O6 S2 O4 115.93(19) . . ?
O6 S2 O5 111.03(17) . . ?
O4 S2 O5 110.93(16) . . ?
O6 S2 C46 107.49(18) . . ?
O4 S2 C46 106.90(18) . . ?
O5 S2 C46 103.68(16) . . ?
O12 S4 O10 114.9(2) . . ?
O12 S4 O11 112.16(17) . . ?
O10 S4 O11 110.2(2) . . ?
O12 S4 C60 105.92(17) . . ?
O10 S4 C60 108.03(18) . . ?
O11 S4 C60 104.96(16) . . ?
C4 N1 C1 109.5(3) . . ?
C8 N2 C11 109.6(3) . . ?
C12 N3 C13 124.4(3) . . ?
C19 N4 C18 125.8(3) . . ?
C23 N5 C20 110.6(3) . . ?
C27 N6 C30 110.1(3) . . ?
C31 N7 C32 122.8(3) . . ?
C38 N8 C37 125.7(3) . . ?
N1 C1 C38 124.7(3) . . ?
N1 C1 C2 107.1(3) . . ?
C38 C1 C2 127.2(3) . . ?
C3 C2 C1 107.4(3) . . ?
C2 C3 C4 108.0(3) . . ?
N1 C4 C3 108.0(3) . . ?
N1 C4 C5 123.1(3) . . ?
C3 C4 C5 128.9(3) . . ?
C8 C5 C4 106.5(3) . . ?
C8 C5 C7 109.6(3) . . ?
C4 C5 C7 112.1(3) . . ?
C8 C5 C6 110.5(3) . . ?
C4 C5 C6 108.5(3) . . ?
C7 C5 C6 109.5(3) . . ?
N2 C8 C9 108.8(3) . . ?
N2 C8 C5 120.2(3) . . ?
C9 C8 C5 131.0(3) . . ?
C10 C9 C8 106.6(3) . . ?
C9 C10 C11 108.6(3) . . ?
N2 C11 C12 125.1(3) . . ?
N2 C11 C10 106.3(3) . . ?
C12 C11 C10 128.1(3) . . ?
N3 C12 C11 125.4(3) . . ?
C18 C13 C14 120.5(4) . . ?
C18 C13 N3 118.9(3) . . ?
C14 C13 N3 120.5(4) . . ?
C15 C14 C13 119.0(4) . . ?
C14 C15 C16 121.1(4) . . ?
C15 C16 C17 120.9(4) . . ?
C16 C17 C18 118.2(4) . . ?
C13 C18 C17 120.2(3) . . ?
C13 C18 N4 119.5(3) . . ?
C17 C18 N4 120.3(4) . . ?
N4 C19 C20 124.9(3) . . ?
C19 C20 N5 126.0(3) . . ?
C19 C20 C21 127.5(3) . . ?
N5 C20 C21 106.4(3) . . ?
C22 C21 C20 107.7(3) . . ?
C21 C22 C23 107.8(3) . . ?
N5 C23 C22 107.6(3) . . ?
N5 C23 C24 124.3(3) . . ?
C22 C23 C24 128.1(3) . . ?
C27 C24 C23 106.5(3) . . ?
C27 C24 C25 110.7(3) . . ?
C23 C24 C25 111.8(3) . . ?
C27 C24 C26 110.6(3) . . ?
C23 C24 C26 108.2(3) . . ?
C25 C24 C26 109.1(3) . . ?
N6 C27 C28 107.6(3) . . ?
N6 C27 C24 121.4(3) . . ?
C28 C27 C24 130.8(3) . . ?
C27 C28 C29 107.9(3) . . ?
C30 C29 C28 107.3(3) . . ?
N6 C30 C31 124.6(3) . . ?
N6 C30 C29 107.0(3) . . ?
C31 C30 C29 128.4(3) . . ?
N7 C31 C30 124.4(3) . . ?
C37 C32 C33 119.4(3) . . ?
C37 C32 N7 118.5(3) . . ?
C33 C32 N7 122.1(3) . . ?
C34 C33 C32 119.3(4) . . ?
C35 C34 C33 120.6(4) . . ?
C34 C35 C36 121.2(4) . . ?
C37 C36 C35 118.5(4) . . ?
C36 C37 C32 121.0(3) . . ?
C36 C37 N8 122.3(3) . . ?
C32 C37 N8 116.8(3) . . ?
N8 C38 C1 124.9(3) . . ?
C44A C39 C40B 104.5(8) . . ?
C44A C39 C40A 119.3(7) . . ?
C40B C39 C40A 14.8(7) . . ?
C44A C39 C44B 13.5(6) . . ?
C40B C39 C44B 117.9(7) . . ?
C40A C39 C44B 132.7(6) . . ?
C44A C39 S1 128.8(6) . . ?
C40B C39 S1 126.5(6) . . ?
C40A C39 S1 111.8(5) . . ?
C44B C39 S1 115.5(4) . . ?
C41A C40A C39 115.5(9) . . ?
C40A C41A C42A 120.3(9) . . ?
C43A C42A C41A 120.8(9) . . ?
C43A C42A C45A 120.6(10) . . ?
C41A C42A C45A 118.6(8) . . ?
C42A C43A C44A 116.6(9) . . ?
C39 C44A C43A 127.4(10) . . ?
C39 C40B C41B 123.1(10) . . ?
C42B C41B C40B 117.5(9) . . ?
C43B C42B C41B 123.0(10) . . ?
C43B C42B C45B 122.0(10) . . ?
C41B C42B C45B 115.0(11) . . ?
C42B C43B C44B 119.4(10) . . ?
C43B C44B C39 119.1(8) . . ?
C51B C46 C47A 103.9(8) . . ?
C51B C46 C51A 14.5(7) . . ?
C47A C46 C51A 118.4(6) . . ?
C51B C46 C47B 118.2(8) . . ?
C47A C46 C47B 14.9(6) . . ?
C51A C46 C47B 132.7(6) . . ?
C51B C46 S2 130.8(7) . . ?
C47A C46 S2 125.1(5) . . ?
C51A C46 S2 116.4(4) . . ?
C47B C46 S2 111.0(5) . . ?
C46 C47A C48A 123.8(8) . . ?
C49A C48A C47A 119.8(8) . . ?
C48A C49A C50A 119.4(8) . . ?
C48A C49A C52A 120.2(10) . . ?
C50A C49A C52A 120.3(8) . . ?
C51A C50A C49A 121.7(8) . . ?
C50A C51A C46 116.8(7) . . ?
C48B C47B C46 113.1(10) . . ?
C49B C48B C47B 124.2(13) . . ?
C50B C49B C48B 122.0(14) . . ?
C50B C49B C52B 113.7(16) . . ?
C48B C49B C52B 124.3(13) . . ?
C49B C50B C51B 115.7(12) . . ?
C46 C51B C50B 126.6(12) . . ?
C65 C60 C61 120.3(4) . . ?
C65 C60 S4 121.1(3) . . ?
C61 C60 S4 118.5(3) . . ?
C62 C61 C60 119.1(4) . . ?
C63 C62 C61 121.8(4) . . ?
C64 C63 C62 118.8(4) . . ?
C64 C63 C66 120.0(4) . . ?
C62 C63 C66 121.2(4) . . ?
C63 C64 C65 120.5(4) . . ?
C60 C65 C64 119.5(4) . . ?
O3M' C3M O3M 64.0(10) . . ?
O10" S3 O102 115.3(9) . . ?
O10" S3 O10' 115.6(9) . . ?
O102 S3 O10' 109.2(6) . . ?
O10" S3 C101 103.3(9) . . ?
O102 S3 C101 105.6(6) . . ?
O10' S3 C101 107.0(7) . . ?
O103 S3' O102 130.7(7) . . ?
O103 S3' O101 117.1(9) . . ?
O102 S3' O101 104.7(9) . . ?
O103 S3' C101 87.3(6) . . ?
O102 S3' C101 103.8(6) . . ?
O101 S3' C101 108.6(9) . . ?
S3 O102 S3' 6.8(6) . . ?
C102 C101 C106 117.7(9) . . ?
C102 C101 S3 118.4(8) . . ?
C106 C101 S3 123.8(8) . . ?
C102 C101 S3' 123.7(8) . . ?
C106 C101 S3' 118.5(8) . . ?
S3 C101 S3' 5.6(5) . . ?
C103 C102 C101 118.5(11) . . ?
C105 C106 C101 124.2(13) . . ?
C102 C103 C104 126.8(13) . . ?
C106 C105 C104 119.5(15) . . ?
C103 C104 C105 112.1(12) . . ?
C103 C104 C107 126.3(14) . . ?
C105 C104 C107 121.6(14) . . ?

_diffrn_measured_fraction_theta_max 0.896
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.106