# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008
data_global
_journal_name_full CrystEngComm
_journal_coden_Cambridge 1350
_publ_contact_author_name 'Christoph Janiak'
_publ_contact_author_email JANIAK@UNI-FREIBURG.DE
_publ_section_title
;
Crystal structure - solid-state CPMAS 13C NMR
correlation in palladacycle pseudo-polymorphs and a vanishing polymorph
;
loop_
_publ_author_name
'Christoph Janiak'
'Anne-Christine Chamayou'
'Natalia Cutillas'
'Anke Hoffmann'
'Karolina Kazmierczak'
;
V.Rodriguez
;
'Jose Ruiz'
# Attachment '1-0.25toluene.cif'
data_vrr171b
_database_code_depnum_ccdc_archive 'CCDC 694832'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Bis{(N,N-dimethylbenzylamine-\kN,\kC)palladium(II)}(\m-acetato-\kO:\kO')
(\m-benzophenone iminato-\kN:\kN) . ~0.25toluene
;
_chemical_name_common
;
Bis((N,N-dimethylbenzylamine-kappaN,kappaC)palladium(ii))(mu-
acetato-kappaO:kappaO') (mu-benzophenone iminato-kappaN:kappaN) .
!0.25toluene
;
_chemical_melting_point ?
_chemical_formula_moiety '2(C33 H37 N3 O2 Pd2), 0.5(C7)'
_chemical_formula_sum 'C69.50 H74 N6 O4 Pd4'
_chemical_formula_weight 1482.95
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_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.2650(10)
_cell_length_b 18.6510(10)
_cell_length_c 18.2170(10)
_cell_angle_alpha 78.708(5)
_cell_angle_beta 81.334(5)
_cell_angle_gamma 75.924(5)
_cell_volume 3298.0(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description prism
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.47
_exptl_crystal_size_mid 0.29
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.493
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1498
_exptl_absorpt_coefficient_mu 1.124
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.6202
_exptl_absorpt_correction_T_max 0.8585
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(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 CCD area diffractometer'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 11962
_diffrn_reflns_av_R_equivalents 0.0184
_diffrn_reflns_av_sigmaI/netI 0.0401
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_theta_min 3.14
_diffrn_reflns_theta_max 25.00
_reflns_number_total 11565
_reflns_number_gt 9237
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker 1997)'
_computing_cell_refinement SMART
_computing_data_reduction 'SAINT (Bruker 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2006)'
_computing_publication_material ?
_publ_section_references
;
Bruker (1997). Smart and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2006). DIAMOND. Version3.1e. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
Each toluene molecule is disordered around the inversion center. The carbon
atoms could only be refined isotropically using the PART (-1, -2) command
for each fragment, no hydrogen atoms could be
calculated. The occupation factors of each toluene add up to approximately
1.75, giving a quarter-occupied toluene at each position or about half
a toluene molecule per asymmetric unit of two independent Pd2 molecules,
that is a quarter toluene molecule per each Pd2 molecule.
For the toluene molecule C71-C75 a sensible geometry was
derived with DFIX commands for the C-C bond lengths. For the final
refinement cycles this geometry was then used as a rigid group
(AFIX 1).
Hydrogen atoms on the acetato methyl groups
C24 and C57
were positioned with a rotating group refinement (AFIX 137).
;
_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^)+(0.0295P)^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 constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 11565
_refine_ls_number_parameters 737
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0388
_refine_ls_R_factor_gt 0.0272
_refine_ls_wR_factor_ref 0.0619
_refine_ls_wR_factor_gt 0.0599
_refine_ls_goodness_of_fit_ref 1.009
_refine_ls_restrained_S_all 1.009
_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 0.66428(3) 1.016376(13) 0.331562(14) 0.01674(6) Uani 1 1 d . . .
Pd2 Pd 0.73676(3) 0.842808(13) 0.333283(14) 0.01819(6) Uani 1 1 d . . .
C1 C 0.4704(3) 1.04987(17) 0.36542(18) 0.0195(7) Uani 1 1 d . . .
C2 C 0.3576(3) 1.04224(18) 0.3361(2) 0.0225(7) Uani 1 1 d . . .
H2 H 0.3696 1.0202 0.2921 0.027 Uiso 1 1 calc R . .
C3 C 0.2272(4) 1.06646(19) 0.3703(2) 0.0272(8) Uani 1 1 d . . .
H3 H 0.1514 1.0609 0.3496 0.033 Uiso 1 1 calc R . .
C4 C 0.2085(4) 1.09864(18) 0.4347(2) 0.0291(8) Uani 1 1 d . . .
H4 H 0.1200 1.1141 0.4588 0.035 Uiso 1 1 calc R . .
C5 C 0.3189(4) 1.10831(19) 0.4639(2) 0.0280(8) Uani 1 1 d . . .
H5 H 0.3061 1.1306 0.5078 0.034 Uiso 1 1 calc R . .
C6 C 0.4477(3) 1.08544(17) 0.42911(18) 0.0215(7) Uani 1 1 d . . .
C7 C 0.5713(3) 1.09301(18) 0.45965(18) 0.0234(8) Uani 1 1 d . . .
H7A H 0.5516 1.1400 0.4809 0.028 Uiso 1 1 calc R . .
H7B H 0.5979 1.0504 0.5003 0.028 Uiso 1 1 calc R . .
C8 C 0.8144(4) 1.0775(2) 0.4285(2) 0.0304(9) Uani 1 1 d . . .
H8A H 0.8287 1.0277 0.4598 0.046 Uiso 1 1 calc R . .
H8B H 0.8136 1.1152 0.4594 0.046 Uiso 1 1 calc R . .
H8C H 0.8876 1.0788 0.3873 0.046 Uiso 1 1 calc R . .
C9 C 0.6639(4) 1.16955(18) 0.3503(2) 0.0267(8) Uani 1 1 d . . .
H9A H 0.5776 1.1813 0.3290 0.040 Uiso 1 1 calc R . .
H9B H 0.7377 1.1705 0.3094 0.040 Uiso 1 1 calc R . .
H9C H 0.6636 1.2068 0.3816 0.040 Uiso 1 1 calc R . .
C10 C 0.6005(3) 0.94281(18) 0.21126(18) 0.0182(7) Uani 1 1 d . . .
C11 C 0.6057(3) 0.87184(17) 0.18198(17) 0.0183(7) Uani 1 1 d . . .
C12 C 0.4899(4) 0.84724(19) 0.17927(19) 0.0256(8) Uani 1 1 d . . .
H12 H 0.4041 0.8765 0.1944 0.031 Uiso 1 1 calc R . .
C13 C 0.4981(4) 0.7798(2) 0.1545(2) 0.0347(9) Uani 1 1 d . . .
H13 H 0.4178 0.7635 0.1532 0.042 Uiso 1 1 calc R . .
C14 C 0.6212(4) 0.7370(2) 0.1319(2) 0.0325(9) Uani 1 1 d . . .
H14 H 0.6265 0.6910 0.1155 0.039 Uiso 1 1 calc R . .
C15 C 0.7373(4) 0.76145(19) 0.13332(19) 0.0277(8) Uani 1 1 d . . .
H15 H 0.8227 0.7325 0.1170 0.033 Uiso 1 1 calc R . .
C16 C 0.7302(4) 0.82797(18) 0.15842(19) 0.0233(8) Uani 1 1 d . . .
H16 H 0.8109 0.8439 0.1596 0.028 Uiso 1 1 calc R . .
C17 C 0.5605(3) 1.01491(18) 0.15767(18) 0.0193(7) Uani 1 1 d . . .
C18 C 0.6192(4) 1.07473(19) 0.15663(19) 0.0258(8) Uani 1 1 d . . .
H18 H 0.6790 1.0714 0.1928 0.031 Uiso 1 1 calc R . .
C19 C 0.5920(4) 1.1397(2) 0.1033(2) 0.0332(9) Uani 1 1 d . . .
H19 H 0.6356 1.1794 0.1024 0.040 Uiso 1 1 calc R . .
C20 C 0.5021(4) 1.1466(2) 0.0517(2) 0.0364(10) Uani 1 1 d . . .
H20 H 0.4817 1.1914 0.0163 0.044 Uiso 1 1 calc R . .
C21 C 0.4416(4) 1.0872(2) 0.0522(2) 0.0336(9) Uani 1 1 d . . .
H21 H 0.3795 1.0913 0.0171 0.040 Uiso 1 1 calc R . .
C22 C 0.4725(4) 1.0219(2) 0.1044(2) 0.0280(8) Uani 1 1 d . . .
H22 H 0.4325 0.9812 0.1036 0.034 Uiso 1 1 calc R . .
C23 C 0.9561(3) 0.93178(19) 0.28787(19) 0.0238(8) Uani 1 1 d . . .
C24 C 1.1068(4) 0.9315(2) 0.2724(2) 0.0386(10) Uani 1 1 d . . .
H24A H 1.1574 0.8820 0.2622 0.058 Uiso 1 1 calc R . .
H24B H 1.1375 0.9426 0.3165 0.058 Uiso 1 1 calc R . .
H24C H 1.1221 0.9696 0.2287 0.058 Uiso 1 1 calc R . .
C25 C 0.5782(4) 0.80249(19) 0.38172(18) 0.0233(8) Uani 1 1 d . . .
C26 C 0.4425(4) 0.8286(2) 0.36959(18) 0.0256(8) Uani 1 1 d . . .
H26 H 0.4166 0.8728 0.3343 0.031 Uiso 1 1 calc R . .
C27 C 0.3444(4) 0.7912(2) 0.4081(2) 0.0360(9) Uani 1 1 d . . .
H27 H 0.2527 0.8101 0.3988 0.043 Uiso 1 1 calc R . .
C28 C 0.3791(5) 0.7265(2) 0.4601(2) 0.0417(11) Uani 1 1 d . . .
H28 H 0.3115 0.7010 0.4858 0.050 Uiso 1 1 calc R . .
C29 C 0.5121(4) 0.6993(2) 0.4743(2) 0.0378(10) Uani 1 1 d . . .
H29 H 0.5363 0.6552 0.5100 0.045 Uiso 1 1 calc R . .
C30 C 0.6105(4) 0.73690(19) 0.43603(19) 0.0287(8) Uani 1 1 d . . .
C31 C 0.7543(4) 0.71311(19) 0.4538(2) 0.0321(9) Uani 1 1 d . . .
H31A H 0.7636 0.7338 0.4983 0.039 Uiso 1 1 calc R . .
H31B H 0.7803 0.6578 0.4658 0.039 Uiso 1 1 calc R . .
C32 C 0.9735(4) 0.7431(2) 0.4127(2) 0.0378(10) Uani 1 1 d . . .
H32A H 0.9561 0.7769 0.4498 0.057 Uiso 1 1 calc R . .
H32B H 1.0324 0.7613 0.3692 0.057 Uiso 1 1 calc R . .
H32C H 1.0176 0.6927 0.4357 0.057 Uiso 1 1 calc R . .
C33 C 0.8731(4) 0.6892(2) 0.3324(2) 0.0354(10) Uani 1 1 d . . .
H33A H 0.7881 0.6870 0.3155 0.053 Uiso 1 1 calc R . .
H33B H 0.9175 0.6389 0.3557 0.053 Uiso 1 1 calc R . .
H33C H 0.9324 0.7075 0.2891 0.053 Uiso 1 1 calc R . .
N1 N 0.6833(3) 1.09404(14) 0.39696(15) 0.0199(6) Uani 1 1 d . . .
N2 N 0.6384(3) 0.93884(14) 0.27577(14) 0.0168(6) Uani 1 1 d . . .
N3 N 0.8447(3) 0.74063(15) 0.38813(16) 0.0262(7) Uani 1 1 d . . .
O1 O 0.8799(2) 0.99120(13) 0.30165(13) 0.0265(5) Uani 1 1 d . . .
O2 O 0.9250(2) 0.87073(13) 0.28558(14) 0.0280(6) Uani 1 1 d . . .
Pd3 Pd 0.86098(2) 0.286151(13) 0.163270(14) 0.01646(6) Uani 1 1 d . . .
Pd4 Pd 0.87709(2) 0.443502(13) 0.178936(14) 0.01571(6) Uani 1 1 d . . .
C34 C 0.8223(3) 0.29360(17) 0.05836(18) 0.0188(7) Uani 1 1 d . . .
C35 C 0.7141(3) 0.33919(19) 0.02231(19) 0.0233(8) Uani 1 1 d . . .
H35 H 0.6489 0.3735 0.0486 0.028 Uiso 1 1 calc R . .
C36 C 0.6991(4) 0.3357(2) -0.0518(2) 0.0301(9) Uani 1 1 d . . .
H36 H 0.6235 0.3670 -0.0750 0.036 Uiso 1 1 calc R . .
C37 C 0.7932(4) 0.2871(2) -0.0912(2) 0.0307(9) Uani 1 1 d . . .
H37 H 0.7833 0.2851 -0.1418 0.037 Uiso 1 1 calc R . .
C38 C 0.9027(4) 0.2411(2) -0.05676(19) 0.0269(8) Uani 1 1 d . . .
H38 H 0.9675 0.2070 -0.0836 0.032 Uiso 1 1 calc R . .
C39 C 0.9178(3) 0.24461(18) 0.01697(19) 0.0223(7) Uani 1 1 d . . .
C40 C 1.0387(3) 0.19899(19) 0.05460(19) 0.0244(8) Uani 1 1 d . . .
H40A H 1.0660 0.1490 0.0390 0.029 Uiso 1 1 calc R . .
H40B H 1.1153 0.2242 0.0394 0.029 Uiso 1 1 calc R . .
C41 C 0.9426(4) 0.1249(2) 0.1636(2) 0.0393(10) Uani 1 1 d . . .
H41A H 0.8600 0.1328 0.1395 0.059 Uiso 1 1 calc R . .
H41B H 0.9203 0.1186 0.2184 0.059 Uiso 1 1 calc R . .
H41C H 1.0064 0.0799 0.1501 0.059 Uiso 1 1 calc R . .
C42 C 1.1286(4) 0.1771(2) 0.1751(2) 0.0357(9) Uani 1 1 d . . .
H42A H 1.1710 0.2202 0.1586 0.054 Uiso 1 1 calc R . .
H42B H 1.1916 0.1319 0.1616 0.054 Uiso 1 1 calc R . .
H42C H 1.1056 0.1706 0.2299 0.054 Uiso 1 1 calc R . .
C43 C 0.6216(3) 0.39970(17) 0.22495(18) 0.0174(7) Uani 1 1 d . . .
C44 C 0.5189(3) 0.35186(17) 0.24492(18) 0.0184(7) Uani 1 1 d . . .
C45 C 0.4275(3) 0.35848(19) 0.30928(19) 0.0242(8) Uani 1 1 d . . .
H45 H 0.4310 0.3934 0.3402 0.029 Uiso 1 1 calc R . .
C46 C 0.3319(4) 0.3152(2) 0.3291(2) 0.0284(8) Uani 1 1 d . . .
H46 H 0.2717 0.3200 0.3738 0.034 Uiso 1 1 calc R . .
C47 C 0.3233(3) 0.2656(2) 0.2848(2) 0.0273(8) Uani 1 1 d . . .
H47 H 0.2573 0.2360 0.2984 0.033 Uiso 1 1 calc R . .
C48 C 0.4120(3) 0.25889(19) 0.2197(2) 0.0269(8) Uani 1 1 d . . .
H48 H 0.4052 0.2252 0.1883 0.032 Uiso 1 1 calc R . .
C49 C 0.5096(3) 0.30049(18) 0.20018(19) 0.0221(7) Uani 1 1 d . . .
H49 H 0.5710 0.2943 0.1561 0.027 Uiso 1 1 calc R . .
C50 C 0.5792(3) 0.47366(17) 0.25376(18) 0.0188(7) Uani 1 1 d . . .
C51 C 0.6467(4) 0.4883(2) 0.3082(2) 0.0290(8) Uani 1 1 d . . .
H51 H 0.7207 0.4516 0.3274 0.035 Uiso 1 1 calc R . .
C52 C 0.6066(4) 0.5559(2) 0.3344(2) 0.0375(10) Uani 1 1 d . . .
H52 H 0.6529 0.5653 0.3718 0.045 Uiso 1 1 calc R . .
C53 C 0.4995(4) 0.6099(2) 0.3065(2) 0.0397(10) Uani 1 1 d . . .
H53 H 0.4732 0.6568 0.3236 0.048 Uiso 1 1 calc R . .
C54 C 0.4316(4) 0.5952(2) 0.2541(2) 0.0368(10) Uani 1 1 d . . .
H54 H 0.3574 0.6320 0.2351 0.044 Uiso 1 1 calc R . .
C55 C 0.4699(4) 0.52762(19) 0.2284(2) 0.0271(8) Uani 1 1 d . . .
H55 H 0.4204 0.5179 0.1927 0.033 Uiso 1 1 calc R . .
C56 C 0.9407(3) 0.31061(18) 0.30870(18) 0.0204(7) Uani 1 1 d . . .
C57 C 0.9655(4) 0.2835(2) 0.39033(19) 0.0296(8) Uani 1 1 d . . .
H57A H 0.9555 0.2315 0.4051 0.044 Uiso 1 1 calc R . .
H57B H 0.8998 0.3152 0.4220 0.044 Uiso 1 1 calc R . .
H57C H 1.0571 0.2862 0.3968 0.044 Uiso 1 1 calc R . .
C58 C 0.8124(3) 0.51670(17) 0.09070(18) 0.0186(7) Uani 1 1 d . . .
C59 C 0.6903(3) 0.52927(19) 0.06022(18) 0.0219(7) Uani 1 1 d . . .
H59 H 0.6271 0.4994 0.0821 0.026 Uiso 1 1 calc R . .
C60 C 0.6599(4) 0.5848(2) -0.0016(2) 0.0279(8) Uani 1 1 d . . .
H60 H 0.5768 0.5919 -0.0219 0.033 Uiso 1 1 calc R . .
C61 C 0.7490(4) 0.62989(19) -0.0339(2) 0.0288(8) Uani 1 1 d . . .
H61 H 0.7266 0.6684 -0.0755 0.035 Uiso 1 1 calc R . .
C62 C 0.8717(4) 0.61855(18) -0.00496(19) 0.0256(8) Uani 1 1 d . . .
H62 H 0.9344 0.6486 -0.0273 0.031 Uiso 1 1 calc R . .
C63 C 0.9020(3) 0.56284(17) 0.05701(18) 0.0201(7) Uani 1 1 d . . .
C64 C 1.0342(3) 0.54662(18) 0.08856(18) 0.0212(7) Uani 1 1 d . . .
H64A H 1.0647 0.5938 0.0848 0.025 Uiso 1 1 calc R . .
H64B H 1.1033 0.5128 0.0595 0.025 Uiso 1 1 calc R . .
C65 C 1.1494(3) 0.4699(2) 0.1948(2) 0.0308(9) Uani 1 1 d . . .
H65A H 1.1914 0.4311 0.1639 0.046 Uiso 1 1 calc R . .
H65B H 1.1363 0.4464 0.2477 0.046 Uiso 1 1 calc R . .
H65C H 1.2081 0.5052 0.1900 0.046 Uiso 1 1 calc R . .
C66 C 0.9556(4) 0.56817(19) 0.2165(2) 0.0302(9) Uani 1 1 d . . .
H66A H 0.8678 0.5955 0.2001 0.045 Uiso 1 1 calc R . .
H66B H 1.0148 0.6032 0.2117 0.045 Uiso 1 1 calc R . .
H66C H 0.9431 0.5443 0.2693 0.045 Uiso 1 1 calc R . .
N4 N 1.0044(3) 0.19037(14) 0.13794(15) 0.0208(6) Uani 1 1 d . . .
N5 N 0.7379(3) 0.38220(14) 0.18837(14) 0.0162(6) Uani 1 1 d . . .
N6 N 1.0174(3) 0.51031(15) 0.16927(15) 0.0214(6) Uani 1 1 d . . .
O3 O 0.9124(2) 0.26380(12) 0.27563(13) 0.0242(5) Uani 1 1 d . . .
O4 O 0.9503(2) 0.37661(12) 0.28171(13) 0.0236(5) Uani 1 1 d . . .
C71 C 0.0619 0.9769 0.0206 0.208 Uiso 0.25 1 d P . .
C72 C 0.0800 1.0248 -0.0462 0.266 Uiso 0.50 1 d P . .
C73 C -0.0021 1.0561 -0.1023 0.198 Uiso 0.25 1 d P . .
C74 C -0.1610 1.0508 -0.0710 0.375 Uiso 0.50 1 d P . .
C75 C -0.1922 1.0089 0.0098 0.204 Uiso 0.25 1 d P . .
C81 C 0.945(5) 0.464(2) 0.440(3) 0.285(18) Uiso 0.50 1 d P A -1
C82 C 1.098(5) 0.491(2) 0.423(3) 0.34(2) Uiso 0.50 1 d P A -1
C83 C 0.897(5) 0.483(3) 0.508(4) 0.36(2) Uiso 0.50 1 d P A -1
C84 C 0.766(6) 0.458(3) 0.520(3) 0.24(3) Uiso 0.25 1 d P 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 0.02032(14) 0.01454(13) 0.01561(13) -0.00396(10) -0.00299(10) -0.00252(10)
Pd2 0.02355(14) 0.01465(13) 0.01618(13) -0.00330(10) -0.00471(11) -0.00172(10)
C1 0.0244(18) 0.0148(16) 0.0170(17) 0.0009(13) -0.0001(14) -0.0042(14)
C2 0.0200(18) 0.0189(17) 0.0280(19) -0.0074(15) -0.0043(15) 0.0007(14)
C3 0.0225(19) 0.0257(19) 0.032(2) -0.0015(16) -0.0055(16) -0.0032(15)
C4 0.025(2) 0.0184(18) 0.038(2) -0.0064(16) 0.0082(17) 0.0020(15)
C5 0.035(2) 0.0224(19) 0.025(2) -0.0087(15) 0.0061(17) -0.0051(16)
C6 0.030(2) 0.0141(16) 0.0194(18) -0.0025(13) 0.0004(15) -0.0051(14)
C7 0.036(2) 0.0186(17) 0.0168(18) -0.0060(14) 0.0000(15) -0.0079(15)
C8 0.032(2) 0.031(2) 0.034(2) -0.0146(17) -0.0101(17) -0.0066(17)
C9 0.035(2) 0.0163(18) 0.029(2) -0.0055(15) 0.0006(17) -0.0082(16)
C10 0.0135(16) 0.0204(17) 0.0204(18) -0.0063(14) 0.0011(14) -0.0027(13)
C11 0.0255(19) 0.0168(17) 0.0132(16) -0.0017(13) -0.0023(14) -0.0065(14)
C12 0.027(2) 0.0265(19) 0.0240(19) -0.0039(15) -0.0044(16) -0.0069(16)
C13 0.040(2) 0.036(2) 0.036(2) -0.0082(18) -0.0097(19) -0.0198(19)
C14 0.055(3) 0.0221(19) 0.026(2) -0.0093(16) -0.0068(19) -0.0136(18)
C15 0.039(2) 0.0198(18) 0.024(2) -0.0080(15) -0.0006(17) -0.0034(16)
C16 0.0267(19) 0.0220(18) 0.0229(19) -0.0056(15) -0.0020(15) -0.0077(15)
C17 0.0206(18) 0.0215(17) 0.0144(17) -0.0051(14) 0.0010(14) -0.0021(14)
C18 0.033(2) 0.0231(18) 0.0210(19) -0.0032(15) -0.0044(16) -0.0058(16)
C19 0.053(3) 0.0207(19) 0.025(2) -0.0022(16) -0.0009(18) -0.0093(18)
C20 0.052(3) 0.026(2) 0.020(2) 0.0010(16) -0.0031(18) 0.0081(18)
C21 0.039(2) 0.034(2) 0.024(2) -0.0037(16) -0.0117(17) 0.0035(18)
C22 0.028(2) 0.028(2) 0.028(2) -0.0057(16) -0.0066(16) -0.0043(16)
C23 0.0255(19) 0.0219(19) 0.0247(19) -0.0014(15) -0.0080(15) -0.0051(15)
C24 0.024(2) 0.034(2) 0.056(3) -0.008(2) -0.0023(19) -0.0041(17)
C25 0.031(2) 0.0254(19) 0.0167(18) -0.0098(14) -0.0001(15) -0.0088(16)
C26 0.035(2) 0.0291(19) 0.0139(17) -0.0065(15) 0.0025(15) -0.0104(16)
C27 0.033(2) 0.047(2) 0.030(2) -0.0143(19) 0.0041(18) -0.0117(19)
C28 0.055(3) 0.040(2) 0.036(2) -0.0095(19) 0.012(2) -0.028(2)
C29 0.064(3) 0.025(2) 0.022(2) 0.0004(16) 0.003(2) -0.012(2)
C30 0.047(2) 0.0221(19) 0.0183(18) -0.0053(15) -0.0048(17) -0.0077(17)
C31 0.052(3) 0.0198(19) 0.022(2) 0.0026(15) -0.0077(18) -0.0062(17)
C32 0.038(2) 0.037(2) 0.036(2) -0.0026(18) -0.0177(19) 0.0017(18)
C33 0.052(3) 0.0226(19) 0.029(2) -0.0115(16) -0.0104(19) 0.0057(18)
N1 0.0281(16) 0.0160(14) 0.0163(14) -0.0041(11) -0.0033(12) -0.0047(12)
N2 0.0188(15) 0.0132(13) 0.0181(15) -0.0042(11) -0.0012(12) -0.0020(11)
N3 0.0364(18) 0.0204(15) 0.0205(16) -0.0052(12) -0.0098(14) 0.0017(13)
O1 0.0230(13) 0.0256(13) 0.0317(14) -0.0083(11) -0.0017(11) -0.0048(11)
O2 0.0252(13) 0.0209(13) 0.0364(15) -0.0053(11) -0.0041(11) -0.0016(10)
Pd3 0.01726(13) 0.01496(13) 0.01740(13) -0.00300(10) -0.00252(10) -0.00335(10)
Pd4 0.01557(13) 0.01489(13) 0.01701(13) -0.00221(10) -0.00319(10) -0.00349(10)
C34 0.0226(18) 0.0175(16) 0.0195(17) -0.0032(13) -0.0020(14) -0.0107(14)
C35 0.0191(18) 0.0294(19) 0.0208(18) -0.0052(15) -0.0008(15) -0.0041(15)
C36 0.023(2) 0.042(2) 0.027(2) -0.0044(17) -0.0071(16) -0.0074(17)
C37 0.032(2) 0.046(2) 0.0210(19) -0.0078(17) -0.0056(17) -0.0179(18)
C38 0.027(2) 0.033(2) 0.026(2) -0.0136(16) 0.0008(16) -0.0107(16)
C39 0.0208(18) 0.0238(18) 0.0244(19) -0.0057(15) 0.0001(15) -0.0094(15)
C40 0.0247(19) 0.0210(18) 0.028(2) -0.0085(15) -0.0010(16) -0.0028(15)
C41 0.045(2) 0.0173(19) 0.051(3) -0.0017(18) 0.009(2) -0.0087(17)
C42 0.024(2) 0.043(2) 0.037(2) -0.0123(19) -0.0091(18) 0.0064(18)
C43 0.0198(18) 0.0150(16) 0.0178(17) -0.0031(13) -0.0044(14) -0.0029(13)
C44 0.0153(17) 0.0191(17) 0.0183(17) 0.0011(14) -0.0021(14) -0.0024(13)
C45 0.030(2) 0.0240(18) 0.0195(18) -0.0048(15) -0.0006(15) -0.0085(15)
C46 0.028(2) 0.033(2) 0.0220(19) -0.0014(16) 0.0076(16) -0.0111(16)
C47 0.0215(19) 0.029(2) 0.032(2) 0.0009(16) -0.0008(16) -0.0117(16)
C48 0.026(2) 0.029(2) 0.030(2) -0.0090(16) -0.0047(16) -0.0084(16)
C49 0.0210(18) 0.0233(18) 0.0216(18) -0.0018(14) 0.0007(15) -0.0074(15)
C50 0.0205(18) 0.0181(17) 0.0172(17) -0.0031(13) 0.0051(14) -0.0072(14)
C51 0.029(2) 0.028(2) 0.030(2) -0.0096(16) -0.0063(17) 0.0000(16)
C52 0.043(3) 0.040(2) 0.035(2) -0.0193(19) -0.0055(19) -0.009(2)
C53 0.053(3) 0.026(2) 0.041(2) -0.0155(18) 0.004(2) -0.0080(19)
C54 0.039(2) 0.024(2) 0.040(2) -0.0029(17) -0.0049(19) 0.0048(17)
C55 0.028(2) 0.028(2) 0.0239(19) 0.0002(16) -0.0038(16) -0.0069(16)
C56 0.0156(17) 0.0239(19) 0.0194(18) -0.0032(15) -0.0016(14) -0.0007(14)
C57 0.039(2) 0.029(2) 0.0210(19) -0.0021(16) -0.0051(17) -0.0082(17)
C58 0.0195(17) 0.0181(17) 0.0170(17) -0.0073(13) 0.0013(14) -0.0006(14)
C59 0.0177(18) 0.0248(18) 0.0215(18) -0.0040(15) -0.0010(14) -0.0018(14)
C60 0.0210(19) 0.031(2) 0.029(2) -0.0067(16) -0.0059(16) 0.0031(16)
C61 0.038(2) 0.0211(18) 0.0211(19) -0.0009(15) -0.0034(17) 0.0026(16)
C62 0.035(2) 0.0174(17) 0.0231(19) -0.0022(15) 0.0010(16) -0.0073(15)
C63 0.0231(18) 0.0170(17) 0.0207(18) -0.0075(14) 0.0002(14) -0.0032(14)
C64 0.0231(18) 0.0211(17) 0.0217(18) -0.0040(14) 0.0028(15) -0.0117(15)
C65 0.023(2) 0.036(2) 0.035(2) -0.0050(17) -0.0092(17) -0.0082(17)
C66 0.043(2) 0.0253(19) 0.028(2) -0.0107(16) -0.0048(17) -0.0121(17)
N4 0.0222(15) 0.0172(14) 0.0232(15) -0.0054(12) -0.0024(12) -0.0031(12)
N5 0.0195(15) 0.0153(13) 0.0142(14) 0.0003(11) -0.0054(12) -0.0051(11)
N6 0.0218(15) 0.0226(15) 0.0220(15) -0.0066(12) -0.0037(12) -0.0061(12)
O3 0.0309(14) 0.0190(12) 0.0219(13) -0.0013(10) -0.0072(11) -0.0031(10)
O4 0.0278(13) 0.0223(13) 0.0224(13) 0.0000(10) -0.0106(11) -0.0067(10)
_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 C1 1.976(3) . ?
Pd1 N2 2.010(2) . ?
Pd1 N1 2.107(3) . ?
Pd1 O1 2.156(2) . ?
Pd1 Pd2 3.1353(4) . ?
Pd2 C25 1.974(3) . ?
Pd2 N2 2.007(2) . ?
Pd2 N3 2.102(3) . ?
Pd2 O2 2.137(2) . ?
C1 C2 1.395(4) . ?
C1 C6 1.409(4) . ?
C2 C3 1.396(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.506(5) . ?
C7 N1 1.495(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N1 1.483(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N1 1.480(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 N2 1.276(4) . ?
C10 C17 1.506(4) . ?
C10 C11 1.508(4) . ?
C11 C12 1.385(4) . ?
C11 C16 1.397(5) . ?
C12 C13 1.397(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.373(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.387(5) . ?
C17 C22 1.391(4) . ?
C18 C19 1.395(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.393(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.392(5) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 O1 1.237(4) . ?
C23 O2 1.265(4) . ?
C23 C24 1.529(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.396(5) . ?
C25 C30 1.419(5) . ?
C26 C27 1.388(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.381(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.392(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.500(5) . ?
C31 N3 1.488(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 N3 1.472(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 N3 1.481(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
Pd3 C34 1.982(3) . ?
Pd3 N5 2.015(3) . ?
Pd3 N4 2.100(3) . ?
Pd3 O3 2.128(2) . ?
Pd3 Pd4 3.0496(4) . ?
Pd4 C58 1.977(3) . ?
Pd4 N5 2.005(2) . ?
Pd4 N6 2.090(3) . ?
Pd4 O4 2.163(2) . ?
C34 C35 1.389(4) . ?
C34 C39 1.405(5) . ?
C35 C36 1.397(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.375(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.388(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.391(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.500(5) . ?
C40 N4 1.492(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 N4 1.475(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 N4 1.479(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N5 1.278(4) . ?
C43 C44 1.502(4) . ?
C43 C50 1.513(4) . ?
C44 C45 1.392(5) . ?
C44 C49 1.402(4) . ?
C45 C46 1.381(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.368(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.388(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.377(4) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C55 1.382(5) . ?
C50 C51 1.393(5) . ?
C51 C52 1.383(5) . ?
C51 H51 0.9500 . ?
C52 C53 1.383(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.367(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.378(5) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 O4 1.255(4) . ?
C56 O3 1.262(4) . ?
C56 C57 1.513(4) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C59 1.396(4) . ?
C58 C63 1.404(4) . ?
C59 C60 1.389(5) . ?
C59 H59 0.9500 . ?
C60 C61 1.381(5) . ?
C60 H60 0.9500 . ?
C61 C62 1.391(5) . ?
C61 H61 0.9500 . ?
C62 C63 1.393(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.494(4) . ?
C64 N6 1.497(4) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 N6 1.475(4) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 N6 1.475(4) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C71 C72 1.3777 . ?
C71 C74 1.4091 2_575 ?
C71 C75 1.4338 2_575 ?
C71 C72 1.4669 2_575 ?
C71 C71 1.5549 2_575 ?
C71 C73 1.5878 2_575 ?
C72 C75 1.3695 2_575 ?
C72 C73 1.3714 . ?
C72 C71 1.4669 2_575 ?
C73 C71 1.5878 2_575 ?
C73 C74 1.6643 . ?
C74 C71 1.4091 2_575 ?
C74 C75 1.5519 . ?
C75 C72 1.3695 2_575 ?
C75 C71 1.4338 2_575 ?
C81 C83 1.34(6) . ?
C81 C82 1.74(5) . ?
C83 C84 1.50(6) . ?
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
C1 Pd1 N2 95.23(12) . . ?
C1 Pd1 N1 82.25(12) . . ?
N2 Pd1 N1 175.83(10) . . ?
C1 Pd1 O1 172.48(11) . . ?
N2 Pd1 O1 92.28(10) . . ?
N1 Pd1 O1 90.28(10) . . ?
C1 Pd1 Pd2 110.12(9) . . ?
N2 Pd1 Pd2 38.66(7) . . ?
N1 Pd1 Pd2 139.32(7) . . ?
O1 Pd1 Pd2 76.19(6) . . ?
C25 Pd2 N2 98.22(13) . . ?
C25 Pd2 N3 83.24(13) . . ?
N2 Pd2 N3 177.01(11) . . ?
C25 Pd2 O2 171.83(12) . . ?
N2 Pd2 O2 89.70(10) . . ?
N3 Pd2 O2 88.76(10) . . ?
C25 Pd2 Pd1 108.11(10) . . ?
N2 Pd2 Pd1 38.72(7) . . ?
N3 Pd2 Pd1 143.24(8) . . ?
O2 Pd2 Pd1 79.36(6) . . ?
C2 C1 C6 117.5(3) . . ?
C2 C1 Pd1 129.4(3) . . ?
C6 C1 Pd1 113.1(2) . . ?
C1 C2 C3 121.1(3) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 119.9(3) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C1 121.4(3) . . ?
C5 C6 C7 122.0(3) . . ?
C1 C6 C7 116.5(3) . . ?
N1 C7 C6 108.7(3) . . ?
N1 C7 H7A 110.0 . . ?
C6 C7 H7A 110.0 . . ?
N1 C7 H7B 110.0 . . ?
C6 C7 H7B 110.0 . . ?
H7A C7 H7B 108.3 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C17 124.1(3) . . ?
N2 C10 C11 119.7(3) . . ?
C17 C10 C11 116.0(3) . . ?
C12 C11 C16 118.2(3) . . ?
C12 C11 C10 121.9(3) . . ?
C16 C11 C10 119.9(3) . . ?
C11 C12 C13 120.7(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C14 C13 C12 120.5(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 119.4(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 120.7(3) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?
C18 C17 C22 118.0(3) . . ?
C18 C17 C10 120.2(3) . . ?
C22 C17 C10 121.6(3) . . ?
C17 C18 C19 121.1(3) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 119.3(3) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C22 C21 C20 119.7(3) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C17 C22 C21 121.5(3) . . ?
C17 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
O1 C23 O2 128.1(3) . . ?
O1 C23 C24 116.3(3) . . ?
O2 C23 C24 115.6(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 116.8(3) . . ?
C26 C25 Pd2 129.6(3) . . ?
C30 C25 Pd2 113.6(3) . . ?
C27 C26 C25 121.4(3) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C28 C27 C26 120.6(4) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C29 C28 C27 119.8(4) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 119.7(4) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C29 C30 C25 121.7(4) . . ?
C29 C30 C31 121.7(3) . . ?
C25 C30 C31 116.5(3) . . ?
N3 C31 C30 109.8(3) . . ?
N3 C31 H31A 109.7 . . ?
C30 C31 H31A 109.7 . . ?
N3 C31 H31B 109.7 . . ?
C30 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C9 N1 C8 108.4(3) . . ?
C9 N1 C7 109.3(3) . . ?
C8 N1 C7 109.6(3) . . ?
C9 N1 Pd1 108.9(2) . . ?
C8 N1 Pd1 114.8(2) . . ?
C7 N1 Pd1 105.62(18) . . ?
C10 N2 Pd2 122.7(2) . . ?
C10 N2 Pd1 133.0(2) . . ?
Pd2 N2 Pd1 102.62(11) . . ?
C32 N3 C33 108.6(3) . . ?
C32 N3 C31 110.0(3) . . ?
C33 N3 C31 109.6(3) . . ?
C32 N3 Pd2 115.7(2) . . ?
C33 N3 Pd2 105.1(2) . . ?
C31 N3 Pd2 107.7(2) . . ?
C23 O1 Pd1 129.5(2) . . ?
C23 O2 Pd2 124.5(2) . . ?
C34 Pd3 N5 99.52(12) . . ?
C34 Pd3 N4 82.68(12) . . ?
N5 Pd3 N4 174.66(10) . . ?
C34 Pd3 O3 172.91(11) . . ?
N5 Pd3 O3 87.22(9) . . ?
N4 Pd3 O3 90.79(10) . . ?
C34 Pd3 Pd4 105.71(9) . . ?
N5 Pd3 Pd4 40.55(7) . . ?
N4 Pd3 Pd4 134.19(7) . . ?
O3 Pd3 Pd4 80.82(6) . . ?
C58 Pd4 N5 96.42(12) . . ?
C58 Pd4 N6 82.57(12) . . ?
N5 Pd4 N6 178.25(11) . . ?
C58 Pd4 O4 172.10(11) . . ?
N5 Pd4 O4 89.27(9) . . ?
N6 Pd4 O4 91.59(9) . . ?
C58 Pd4 Pd3 110.41(9) . . ?
N5 Pd4 Pd3 40.78(7) . . ?
N6 Pd4 Pd3 140.93(8) . . ?
O4 Pd4 Pd3 77.46(6) . . ?
C35 C34 C39 117.4(3) . . ?
C35 C34 Pd3 128.6(3) . . ?
C39 C34 Pd3 113.9(2) . . ?
C34 C35 C36 121.5(3) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C37 C36 C35 120.2(3) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C36 C37 C38 119.6(3) . . ?
C36 C37 H37 120.2 . . ?
C38 C37 H37 120.2 . . ?
C37 C38 C39 120.2(3) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 . . ?
C38 C39 C34 121.1(3) . . ?
C38 C39 C40 121.7(3) . . ?
C34 C39 C40 117.2(3) . . ?
N4 C40 C39 109.2(3) . . ?
N4 C40 H40A 109.8 . . ?
C39 C40 H40A 109.8 . . ?
N4 C40 H40B 109.8 . . ?
C39 C40 H40B 109.8 . . ?
H40A C40 H40B 108.3 . . ?
N4 C41 H41A 109.5 . . ?
N4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N4 C42 H42A 109.5 . . ?
N4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C43 C44 125.8(3) . . ?
N5 C43 C50 119.8(3) . . ?
C44 C43 C50 114.5(3) . . ?
C45 C44 C49 117.8(3) . . ?
C45 C44 C43 119.9(3) . . ?
C49 C44 C43 122.3(3) . . ?
C46 C45 C44 121.3(3) . . ?
C46 C45 H45 119.4 . . ?
C44 C45 H45 119.4 . . ?
C47 C46 C45 120.4(3) . . ?
C47 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C46 C47 C48 119.3(3) . . ?
C46 C47 H47 120.3 . . ?
C48 C47 H47 120.3 . . ?
C49 C48 C47 120.8(3) . . ?
C49 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
C48 C49 C44 120.3(3) . . ?
C48 C49 H49 119.8 . . ?
C44 C49 H49 119.8 . . ?
C55 C50 C51 118.2(3) . . ?
C55 C50 C43 120.8(3) . . ?
C51 C50 C43 121.0(3) . . ?
C52 C51 C50 120.5(3) . . ?
C52 C51 H51 119.7 . . ?
C50 C51 H51 119.7 . . ?
C53 C52 C51 120.2(4) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C54 C53 C52 119.5(4) . . ?
C54 C53 H53 120.3 . . ?
C52 C53 H53 120.3 . . ?
C53 C54 C55 120.6(4) . . ?
C53 C54 H54 119.7 . . ?
C55 C54 H54 119.7 . . ?
C54 C55 C50 121.0(3) . . ?
C54 C55 H55 119.5 . . ?
C50 C55 H55 119.5 . . ?
O4 C56 O3 127.5(3) . . ?
O4 C56 C57 116.7(3) . . ?
O3 C56 C57 115.8(3) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C59 C58 C63 117.4(3) . . ?
C59 C58 Pd4 128.7(2) . . ?
C63 C58 Pd4 113.8(2) . . ?
C60 C59 C58 121.0(3) . . ?
C60 C59 H59 119.5 . . ?
C58 C59 H59 119.5 . . ?
C61 C60 C59 120.8(3) . . ?
C61 C60 H60 119.6 . . ?
C59 C60 H60 119.6 . . ?
C60 C61 C62 119.5(3) . . ?
C60 C61 H61 120.2 . . ?
C62 C61 H61 120.2 . . ?
C61 C62 C63 119.6(3) . . ?
C61 C62 H62 120.2 . . ?
C63 C62 H62 120.2 . . ?
C62 C63 C58 121.6(3) . . ?
C62 C63 C64 121.7(3) . . ?
C58 C63 C64 116.6(3) . . ?
C63 C64 N6 109.0(3) . . ?
C63 C64 H64A 109.9 . . ?
N6 C64 H64A 109.9 . . ?
C63 C64 H64B 109.9 . . ?
N6 C64 H64B 109.9 . . ?
H64A C64 H64B 108.3 . . ?
N6 C65 H65A 109.5 . . ?
N6 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
N6 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
N6 C66 H66A 109.5 . . ?
N6 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
N6 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C41 N4 C42 108.5(3) . . ?
C41 N4 C40 108.9(3) . . ?
C42 N4 C40 109.9(3) . . ?
C41 N4 Pd3 108.1(2) . . ?
C42 N4 Pd3 112.9(2) . . ?
C40 N4 Pd3 108.45(19) . . ?
C43 N5 Pd4 121.9(2) . . ?
C43 N5 Pd3 135.3(2) . . ?
Pd4 N5 Pd3 98.67(11) . . ?
C66 N6 C65 108.7(3) . . ?
C66 N6 C64 109.5(3) . . ?
C65 N6 C64 110.7(3) . . ?
C66 N6 Pd4 105.8(2) . . ?
C65 N6 Pd4 114.5(2) . . ?
C64 N6 Pd4 107.37(18) . . ?
C56 O3 Pd3 125.1(2) . . ?
C56 O4 Pd4 127.3(2) . . ?
C72 C71 C74 123.4 . 2_575 ?
C72 C71 C75 58.3 . 2_575 ?
C74 C71 C75 66.2 2_575 2_575 ?
C72 C71 C72 113.8 . 2_575 ?
C74 C71 C72 120.3 2_575 2_575 ?
C75 C71 C72 170.6 2_575 2_575 ?
C72 C71 C71 59.7 . 2_575 ?
C74 C71 C71 164.7 2_575 2_575 ?
C75 C71 C71 117.7 2_575 2_575 ?
C72 C71 C71 54.2 2_575 2_575 ?
C72 C71 C73 161.5 . 2_575 ?
C74 C71 C73 67.2 2_575 2_575 ?
C75 C71 C73 133.0 2_575 2_575 ?
C72 C71 C73 53.2 2_575 2_575 ?
C71 C71 C73 106.0 2_575 2_575 ?
C75 C72 C73 161.6 2_575 . ?
C75 C72 C71 62.9 2_575 . ?
C73 C72 C71 131.8 . . ?
C75 C72 C71 128.8 2_575 2_575 ?
C73 C72 C71 67.9 . 2_575 ?
C71 C72 C71 66.2 . 2_575 ?
C72 C73 C71 58.9 . 2_575 ?
C72 C73 C74 110.2 . . ?
C71 C73 C74 51.3 2_575 . ?
C71 C74 C75 57.7 2_575 . ?
C71 C74 C73 61.6 2_575 . ?
C75 C74 C73 119.0 . . ?
C72 C75 C71 58.8 2_575 2_575 ?
C72 C75 C74 114.1 2_575 . ?
C71 C75 C74 56.2 2_575 . ?
C83 C81 C82 102(4) . . ?
C81 C83 C84 100(6) . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 0.385
_refine_diff_density_min -0.463
_refine_diff_density_rms 0.076
# Attachment '1-1.5benzene.CIF'
data_c6h6171a
_database_code_depnum_ccdc_archive 'CCDC 694833'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Bis{(N,N-dimethylbenzylamine-\kN,\kC)palladium(II)}(\m-acetato-\kO:\kO')
(\m-benzophenone iminato-\kN:\kN) . 1.5benzene
;
_chemical_name_common
;
Bis((N,N-dimethylbenzylamine-kappaN,kappaC)palladium(ii))(mu-
acetato-kappaO:kappaO') (mu-benzophenone iminato-kappaN:kappaN) .
1.5benzene
;
_chemical_melting_point ?
_chemical_formula_moiety 'C33 H37 N3 O2 Pd2, 0.5 (C12 H12), 0.5(C6 H6)'
_chemical_formula_sum 'C42 H46 N3 O2 Pd2'
_chemical_formula_weight 837.62
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'
Pd Pd -0.9988 1.0072 '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_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.3712(5)
_cell_length_b 11.2535(7)
_cell_length_c 18.6983(11)
_cell_angle_alpha 83.304(3)
_cell_angle_beta 84.253(3)
_cell_angle_gamma 78.682(3)
_cell_volume 1914.31(19)
_cell_formula_units_Z 2
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used 9695
_cell_measurement_theta_min 2.25
_cell_measurement_theta_max 31.36
_exptl_crystal_description isometric
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.453
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 854
_exptl_absorpt_coefficient_mu 0.977
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8285
_exptl_absorpt_correction_T_max 0.9500
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 203(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 APEXII AXS CCD diffractometer'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 30419
_diffrn_reflns_av_R_equivalents 0.0275
_diffrn_reflns_av_sigmaI/netI 0.0270
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 1.85
_diffrn_reflns_theta_max 26.35
_reflns_number_total 7746
_reflns_number_gt 6641
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2006)'
_computing_publication_material ?
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2006). DIAMOND. Version 3.1e. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
One benzene molecule is situated around the inversion center with only half
the molecule being part of the asymmetric unit.
The other benzene molecule is rotationally disordered around its pseudo-six-
fold axis. Two benzene moieties rotated by 30 deg could be discerned.
Two half-occuped positions were refined for each carbon atom using a riding
model (AFIX 66/65) and two PART (1,2) commands.
For both benzene molecules the carbon atoms were refined anisotropically and
their hydrogen atoms calculated.
;
_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^)+(0.0223P)^2^+0.8440P] 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 7746
_refine_ls_number_parameters 473
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0309
_refine_ls_R_factor_gt 0.0231
_refine_ls_wR_factor_ref 0.0548
_refine_ls_wR_factor_gt 0.0519
_refine_ls_goodness_of_fit_ref 1.034
_refine_ls_restrained_S_all 1.034
_refine_ls_shift/su_max 0.002
_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 0.391614(17) 0.537691(13) 0.341565(8) 0.02634(5) Uani 1 1 d . . .
Pd2 Pd 0.474841(17) 0.270139(13) 0.304645(8) 0.02596(5) Uani 1 1 d . . .
C1 C 0.5480(2) 0.60873(18) 0.37291(11) 0.0297(4) Uani 1 1 d . . .
C2 C 0.6842(2) 0.6173(2) 0.33751(12) 0.0355(5) Uani 1 1 d . . .
H2 H 0.7100 0.5862 0.2925 0.043 Uiso 1 1 calc R . .
C3 C 0.7823(3) 0.6709(2) 0.36748(14) 0.0430(6) Uani 1 1 d . . .
H3 H 0.8735 0.6765 0.3426 0.052 Uiso 1 1 calc R . .
C4 C 0.7461(3) 0.7159(2) 0.43388(15) 0.0473(6) Uani 1 1 d . . .
H4 H 0.8136 0.7503 0.4548 0.057 Uiso 1 1 calc R . .
C5 C 0.6117(3) 0.7106(2) 0.46942(14) 0.0444(6) Uani 1 1 d . . .
H5 H 0.5870 0.7422 0.5143 0.053 Uiso 1 1 calc R . .
C6 C 0.5121(2) 0.65865(19) 0.43906(11) 0.0337(5) Uani 1 1 d . . .
C7 C 0.3651(3) 0.6489(2) 0.47631(12) 0.0387(5) Uani 1 1 d . . .
H7A H 0.3740 0.5783 0.5127 0.046 Uiso 1 1 calc R . .
H7B H 0.3253 0.7221 0.5007 0.046 Uiso 1 1 calc R . .
N1 N 0.26514(19) 0.63502(15) 0.42171(9) 0.0315(4) Uani 1 1 d . . .
C8 C 0.1450(3) 0.5774(2) 0.45794(13) 0.0437(6) Uani 1 1 d . . .
H8A H 0.0832 0.5641 0.4221 0.066 Uiso 1 1 calc R . .
H8B H 0.0877 0.6303 0.4919 0.066 Uiso 1 1 calc R . .
H8C H 0.1851 0.4999 0.4835 0.066 Uiso 1 1 calc R . .
C9 C 0.2022(3) 0.7551(2) 0.38585(13) 0.0434(6) Uani 1 1 d . . .
H9A H 0.2798 0.7924 0.3600 0.065 Uiso 1 1 calc R . .
H9B H 0.1511 0.8069 0.4219 0.065 Uiso 1 1 calc R . .
H9C H 0.1344 0.7449 0.3521 0.065 Uiso 1 1 calc R . .
N2 N 0.50791(18) 0.43711(15) 0.26763(9) 0.0260(4) Uani 1 1 d . . .
C10 C 0.5485(2) 0.46756(18) 0.20202(10) 0.0275(4) Uani 1 1 d . . .
C11 C 0.5509(2) 0.59690(19) 0.17346(10) 0.0322(5) Uani 1 1 d . . .
C12 C 0.4315(3) 0.6891(2) 0.18570(12) 0.0418(6) Uani 1 1 d . . .
H12 H 0.3457 0.6703 0.2111 0.050 Uiso 1 1 calc R . .
C13 C 0.4386(4) 0.8084(2) 0.16066(14) 0.0564(8) Uani 1 1 d . . .
H13 H 0.3569 0.8701 0.1686 0.068 Uiso 1 1 calc R . .
C14 C 0.5631(4) 0.8375(2) 0.12443(15) 0.0657(9) Uani 1 1 d . . .
H14 H 0.5677 0.9191 0.1085 0.079 Uiso 1 1 calc R . .
C15 C 0.6823(4) 0.7463(3) 0.11128(14) 0.0594(8) Uani 1 1 d . . .
H15 H 0.7680 0.7661 0.0863 0.071 Uiso 1 1 calc R . .
C16 C 0.6757(3) 0.6262(2) 0.13485(12) 0.0420(6) Uani 1 1 d . . .
H16 H 0.7559 0.5643 0.1247 0.050 Uiso 1 1 calc R . .
C17 C 0.5879(2) 0.37571(19) 0.14746(10) 0.0302(5) Uani 1 1 d . . .
C18 C 0.5128(3) 0.3966(2) 0.08570(12) 0.0428(6) Uani 1 1 d . . .
H18 H 0.4469 0.4703 0.0770 0.051 Uiso 1 1 calc R . .
C19 C 0.5335(3) 0.3109(2) 0.03691(14) 0.0539(7) Uani 1 1 d . . .
H19 H 0.4800 0.3256 -0.0042 0.065 Uiso 1 1 calc R . .
C20 C 0.6318(3) 0.2044(2) 0.04810(13) 0.0519(7) Uani 1 1 d . . .
H20 H 0.6453 0.1456 0.0150 0.062 Uiso 1 1 calc R . .
C21 C 0.7108(3) 0.1836(2) 0.10805(13) 0.0501(7) Uani 1 1 d . . .
H21 H 0.7803 0.1116 0.1150 0.060 Uiso 1 1 calc R . .
C22 C 0.6885(3) 0.2682(2) 0.15801(12) 0.0398(5) Uani 1 1 d . . .
H22 H 0.7417 0.2529 0.1992 0.048 Uiso 1 1 calc R . .
O1 O 0.19777(17) 0.49536(15) 0.30592(9) 0.0417(4) Uani 1 1 d . . .
O2 O 0.26784(17) 0.31567(14) 0.26020(8) 0.0374(4) Uani 1 1 d . . .
C23 C 0.1814(2) 0.4145(2) 0.26862(11) 0.0331(5) Uani 1 1 d . . .
C24 C 0.0429(3) 0.4403(2) 0.22993(14) 0.0460(6) Uani 1 1 d . . .
H24A H 0.0366 0.3701 0.2057 0.069 Uiso 1 1 calc R . .
H24B H 0.0440 0.5105 0.1946 0.069 Uiso 1 1 calc R . .
H24C H -0.0408 0.4567 0.2647 0.069 Uiso 1 1 calc R . .
C25 C 0.6630(2) 0.21713(18) 0.34836(10) 0.0278(4) Uani 1 1 d . . .
C26 C 0.7803(2) 0.2771(2) 0.34369(11) 0.0325(5) Uani 1 1 d . . .
H26 H 0.7737 0.3539 0.3170 0.039 Uiso 1 1 calc R . .
C27 C 0.9066(3) 0.2269(2) 0.37724(12) 0.0385(5) Uani 1 1 d . . .
H27 H 0.9842 0.2697 0.3731 0.046 Uiso 1 1 calc R . .
C28 C 0.9192(3) 0.1144(2) 0.41678(12) 0.0435(6) Uani 1 1 d . . .
H28 H 1.0054 0.0799 0.4390 0.052 Uiso 1 1 calc R . .
C29 C 0.8044(3) 0.0531(2) 0.42341(13) 0.0426(6) Uani 1 1 d . . .
H29 H 0.8121 -0.0233 0.4506 0.051 Uiso 1 1 calc R . .
C30 C 0.6771(2) 0.10352(19) 0.39007(11) 0.0341(5) Uani 1 1 d . . .
C31 C 0.5448(3) 0.0455(2) 0.40036(12) 0.0406(6) Uani 1 1 d . . .
H31A H 0.5746 -0.0431 0.4013 0.049 Uiso 1 1 calc R . .
H31B H 0.4908 0.0639 0.4466 0.049 Uiso 1 1 calc R . .
N3 N 0.4491(2) 0.09205(15) 0.34054(10) 0.0334(4) Uani 1 1 d . . .
C32 C 0.2968(3) 0.0830(2) 0.36587(15) 0.0510(7) Uani 1 1 d . . .
H32A H 0.2653 0.1312 0.4063 0.077 Uiso 1 1 calc R . .
H32B H 0.2909 -0.0014 0.3810 0.077 Uiso 1 1 calc R . .
H32C H 0.2342 0.1134 0.3269 0.077 Uiso 1 1 calc R . .
C33 C 0.4970(3) 0.0192(2) 0.27852(14) 0.0550(7) Uani 1 1 d . . .
H33A H 0.5981 0.0228 0.2630 0.083 Uiso 1 1 calc R . .
H33B H 0.4365 0.0518 0.2390 0.083 Uiso 1 1 calc R . .
H33C H 0.4877 -0.0648 0.2929 0.083 Uiso 1 1 calc R . .
C34 C -0.0097(4) 0.3820(4) 0.02386(19) 0.0802(10) Uani 1 1 d . . .
H34 H -0.0154 0.3008 0.0404 0.096 Uiso 1 1 calc R . .
C35 C 0.1175(4) 0.5470(4) 0.0133(2) 0.0824(10) Uani 1 1 d . . .
H35 H 0.1988 0.5786 0.0225 0.099 Uiso 1 1 calc R . .
C36 C 0.1077(4) 0.4295(4) 0.03712(19) 0.0837(11) Uani 1 1 d . . .
H36 H 0.1825 0.3804 0.0630 0.100 Uiso 1 1 calc R . .
C41 C 0.0667(17) 0.9174(14) 0.0980(7) 0.095(4) Uani 0.50 1 d PG A 1
H41 H 0.0804 0.8775 0.0557 0.114 Uiso 0.50 1 calc PR A 1
C42 C 0.1178(12) 1.0252(14) 0.0986(4) 0.084(4) Uani 0.50 1 d PG A 1
H42 H 0.1661 1.0581 0.0567 0.101 Uiso 0.50 1 calc PR A 1
C43 C 0.0975(11) 1.0842(6) 0.1611(8) 0.091(4) Uani 0.50 1 d PG A 1
H43 H 0.1321 1.1570 0.1615 0.109 Uiso 0.50 1 calc PR A 1
C44 C 0.0260(11) 1.0354(13) 0.2231(4) 0.082(4) Uani 0.50 1 d PG A 1
H44 H 0.0123 1.0753 0.2654 0.098 Uiso 0.50 1 calc PR A 1
C45 C -0.0251(8) 0.9277(13) 0.2225(6) 0.090(4) Uani 0.50 1 d PG A 1
H45 H -0.0734 0.8947 0.2644 0.107 Uiso 0.50 1 calc PR A 1
C46 C -0.0048(14) 0.8687(6) 0.1599(11) 0.111(5) Uani 0.50 1 d PG A 1
H46 H -0.0393 0.7958 0.1595 0.133 Uiso 0.50 1 calc PR A 1
C51 C 0.1131(15) 0.9868(16) 0.0837(4) 0.101(5) Uani 0.50 1 d PG B 2
H51 H 0.1508 0.9867 0.0352 0.121 Uiso 0.50 1 calc PR B 2
C52 C 0.1289(11) 1.0794(9) 0.1237(11) 0.110(5) Uani 0.50 1 d PG B 2
H52 H 0.1773 1.1419 0.1022 0.132 Uiso 0.50 1 calc PR B 2
C53 C 0.0731(17) 1.0797(9) 0.1954(10) 0.100(6) Uani 0.50 1 d PG B 2
H53 H 0.0838 1.1423 0.2225 0.120 Uiso 0.50 1 calc PR B 2
C54 C 0.0016(15) 0.9873(16) 0.2272(3) 0.091(5) Uani 0.50 1 d PG B 2
H54 H -0.0361 0.9874 0.2757 0.109 Uiso 0.50 1 calc PR B 2
C55 C -0.0142(11) 0.8947(10) 0.1872(8) 0.105(4) Uani 0.50 1 d PG B 2
H55 H -0.0626 0.8322 0.2086 0.126 Uiso 0.50 1 calc PR B 2
C56 C 0.0415(17) 0.8944(10) 0.1154(7) 0.127(7) Uani 0.50 1 d PG B 2
H56 H 0.0308 0.8318 0.0884 0.152 Uiso 0.50 1 calc PR B 2
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 0.02603(9) 0.02527(8) 0.02766(8) -0.00348(6) -0.00166(6) -0.00439(6)
Pd2 0.02638(9) 0.02496(8) 0.02688(8) -0.00264(6) -0.00311(6) -0.00509(6)
C1 0.0320(12) 0.0236(10) 0.0327(10) 0.0001(8) -0.0087(9) -0.0020(9)
C2 0.0350(13) 0.0350(12) 0.0369(11) -0.0004(9) -0.0074(10) -0.0070(10)
C3 0.0333(14) 0.0399(13) 0.0570(15) 0.0012(11) -0.0108(11) -0.0096(11)
C4 0.0415(15) 0.0326(12) 0.0733(18) -0.0122(12) -0.0281(13) -0.0040(11)
C5 0.0464(15) 0.0348(12) 0.0539(14) -0.0176(11) -0.0201(12) 0.0033(11)
C6 0.0355(13) 0.0273(11) 0.0364(11) -0.0047(9) -0.0114(10) 0.0038(9)
C7 0.0397(14) 0.0409(13) 0.0343(11) -0.0109(10) -0.0064(10) 0.0015(10)
N1 0.0306(10) 0.0280(9) 0.0338(9) -0.0037(7) -0.0018(8) -0.0002(8)
C8 0.0370(14) 0.0459(14) 0.0444(13) -0.0043(11) 0.0075(11) -0.0042(11)
C9 0.0445(15) 0.0303(12) 0.0513(14) -0.0028(10) -0.0076(12) 0.0039(10)
N2 0.0222(9) 0.0278(9) 0.0280(8) -0.0017(7) -0.0063(7) -0.0029(7)
C10 0.0240(11) 0.0296(10) 0.0286(10) -0.0009(8) -0.0075(8) -0.0028(9)
C11 0.0414(14) 0.0316(11) 0.0248(10) 0.0011(8) -0.0124(9) -0.0070(10)
C12 0.0533(16) 0.0361(12) 0.0350(12) -0.0015(10) -0.0139(11) -0.0016(11)
C13 0.091(2) 0.0322(13) 0.0450(14) -0.0017(11) -0.0262(15) -0.0002(14)
C14 0.124(3) 0.0338(14) 0.0467(15) 0.0061(12) -0.0277(18) -0.0293(17)
C15 0.084(2) 0.0616(19) 0.0443(14) 0.0064(13) -0.0117(15) -0.0448(18)
C16 0.0509(16) 0.0451(14) 0.0332(12) 0.0026(10) -0.0097(11) -0.0173(12)
C17 0.0324(12) 0.0321(11) 0.0257(10) -0.0012(8) -0.0023(9) -0.0059(9)
C18 0.0513(16) 0.0378(13) 0.0390(12) -0.0038(10) -0.0180(11) -0.0006(11)
C19 0.070(2) 0.0548(16) 0.0403(13) -0.0094(12) -0.0229(13) -0.0087(14)
C20 0.0685(19) 0.0468(15) 0.0410(14) -0.0170(11) -0.0040(13) -0.0046(14)
C21 0.0555(17) 0.0456(14) 0.0424(14) -0.0104(11) -0.0038(13) 0.0107(12)
C22 0.0406(14) 0.0429(13) 0.0305(11) -0.0044(9) -0.0057(10) 0.0069(11)
O1 0.0289(9) 0.0476(10) 0.0516(10) -0.0185(8) -0.0034(7) -0.0061(7)
O2 0.0319(9) 0.0346(8) 0.0478(9) -0.0061(7) -0.0119(7) -0.0056(7)
C23 0.0281(12) 0.0387(12) 0.0332(11) 0.0003(9) -0.0021(9) -0.0107(10)
C24 0.0366(14) 0.0502(15) 0.0524(14) -0.0038(12) -0.0142(12) -0.0061(12)
C25 0.0289(11) 0.0306(10) 0.0228(9) -0.0024(8) -0.0032(8) -0.0022(9)
C26 0.0317(12) 0.0348(11) 0.0298(10) 0.0015(9) -0.0051(9) -0.0045(10)
C27 0.0310(13) 0.0486(14) 0.0363(12) -0.0029(10) -0.0054(10) -0.0078(11)
C28 0.0348(14) 0.0545(15) 0.0378(12) 0.0020(11) -0.0109(11) 0.0004(12)
C29 0.0461(15) 0.0376(13) 0.0403(13) 0.0042(10) -0.0098(11) -0.0005(11)
C30 0.0350(13) 0.0322(11) 0.0337(11) -0.0026(9) -0.0037(10) -0.0033(10)
C31 0.0482(15) 0.0294(11) 0.0426(13) 0.0033(10) -0.0048(11) -0.0066(10)
N3 0.0340(11) 0.0258(9) 0.0413(10) -0.0049(8) -0.0022(8) -0.0076(8)
C32 0.0427(15) 0.0396(14) 0.0729(18) -0.0011(12) 0.0005(13) -0.0180(12)
C33 0.076(2) 0.0375(14) 0.0557(16) -0.0178(12) -0.0044(14) -0.0142(13)
C34 0.076(3) 0.082(2) 0.073(2) 0.0044(19) 0.016(2) -0.009(2)
C35 0.058(2) 0.105(3) 0.082(2) -0.003(2) 0.0030(19) -0.018(2)
C36 0.062(2) 0.111(3) 0.068(2) 0.004(2) -0.0024(18) -0.001(2)
C41 0.092(10) 0.079(8) 0.114(9) -0.046(7) -0.035(8) 0.019(7)
C42 0.091(7) 0.066(8) 0.082(6) -0.042(6) -0.018(5) 0.044(7)
C43 0.121(9) 0.083(6) 0.057(8) -0.037(6) -0.043(9) 0.045(6)
C44 0.111(9) 0.058(9) 0.067(6) 0.002(5) -0.044(6) 0.020(7)
C45 0.092(7) 0.071(8) 0.112(10) -0.025(6) -0.064(7) 0.007(7)
C46 0.106(10) 0.121(9) 0.119(12) -0.074(10) -0.073(10) 0.017(7)
C51 0.100(9) 0.084(11) 0.111(8) -0.062(8) -0.037(7) 0.046(8)
C52 0.122(10) 0.070(8) 0.124(14) -0.027(8) -0.057(12) 0.051(7)
C53 0.160(16) 0.063(7) 0.067(9) -0.028(7) -0.076(10) 0.050(8)
C54 0.122(12) 0.072(11) 0.074(6) -0.031(6) -0.035(6) 0.023(8)
C55 0.108(8) 0.112(10) 0.109(10) -0.059(7) -0.064(9) 0.004(7)
C56 0.095(12) 0.188(17) 0.095(10) -0.094(12) -0.044(9) 0.043(11)
_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 C1 1.968(2) . ?
Pd1 N2 1.9898(16) . ?
Pd1 N1 2.0899(16) . ?
Pd1 O1 2.1510(16) . ?
Pd1 Pd2 3.0993(3) . ?
Pd2 C25 1.973(2) . ?
Pd2 N2 1.9970(16) . ?
Pd2 N3 2.0902(17) . ?
Pd2 O2 2.1330(15) . ?
C1 C2 1.393(3) . ?
C1 C6 1.401(3) . ?
C2 C3 1.386(3) . ?
C2 H2 0.9400 . ?
C3 C4 1.382(3) . ?
C3 H3 0.9400 . ?
C4 C5 1.372(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.391(3) . ?
C5 H5 0.9400 . ?
C6 C7 1.498(3) . ?
C7 N1 1.493(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
N1 C9 1.476(3) . ?
N1 C8 1.476(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
N2 C10 1.276(2) . ?
C10 C11 1.494(3) . ?
C10 C17 1.505(3) . ?
C11 C16 1.388(3) . ?
C11 C12 1.388(3) . ?
C12 C13 1.381(3) . ?
C12 H12 0.9400 . ?
C13 C14 1.366(4) . ?
C13 H13 0.9400 . ?
C14 C15 1.384(4) . ?
C14 H14 0.9400 . ?
C15 C16 1.383(4) . ?
C15 H15 0.9400 . ?
C16 H16 0.9400 . ?
C17 C18 1.385(3) . ?
C17 C22 1.388(3) . ?
C18 C19 1.377(3) . ?
C18 H18 0.9400 . ?
C19 C20 1.370(4) . ?
C19 H19 0.9400 . ?
C20 C21 1.377(4) . ?
C20 H20 0.9400 . ?
C21 C22 1.383(3) . ?
C21 H21 0.9400 . ?
C22 H22 0.9400 . ?
O1 C23 1.249(3) . ?
O2 C23 1.257(3) . ?
C23 C24 1.512(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 C26 1.389(3) . ?
C25 C30 1.408(3) . ?
C26 C27 1.385(3) . ?
C26 H26 0.9400 . ?
C27 C28 1.380(3) . ?
C27 H27 0.9400 . ?
C28 C29 1.376(3) . ?
C28 H28 0.9400 . ?
C29 C30 1.391(3) . ?
C29 H29 0.9400 . ?
C30 C31 1.497(3) . ?
C31 N3 1.486(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
N3 C32 1.477(3) . ?
N3 C33 1.480(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C34 C35 1.355(5) 2_565 ?
C34 C36 1.369(5) . ?
C34 H34 0.9400 . ?
C35 C34 1.355(5) 2_565 ?
C35 C36 1.363(5) . ?
C35 H35 0.9400 . ?
C36 H36 0.9400 . ?
C41 C42 1.3900 . ?
C41 C46 1.3900 . ?
C41 H41 0.9400 . ?
C42 C43 1.3900 . ?
C42 H42 0.9400 . ?
C43 C44 1.3900 . ?
C43 H43 0.9400 . ?
C44 C45 1.3900 . ?
C44 H44 0.9400 . ?
C45 C46 1.3900 . ?
C45 H45 0.9400 . ?
C46 H46 0.9400 . ?
C51 C52 1.3900 . ?
C51 C56 1.3900 . ?
C51 H51 0.9400 . ?
C52 C53 1.3900 . ?
C52 H52 0.9400 . ?
C53 C54 1.3900 . ?
C53 H53 0.9400 . ?
C54 C55 1.3900 . ?
C54 H54 0.9400 . ?
C55 C56 1.3900 . ?
C55 H55 0.9400 . ?
C56 H56 0.9400 . ?
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
C1 Pd1 N2 99.07(8) . . ?
C1 Pd1 N1 82.86(8) . . ?
N2 Pd1 N1 176.92(6) . . ?
C1 Pd1 O1 169.00(7) . . ?
N2 Pd1 O1 88.32(6) . . ?
N1 Pd1 O1 90.11(6) . . ?
C1 Pd1 Pd2 116.68(6) . . ?
N2 Pd1 Pd2 39.06(5) . . ?
N1 Pd1 Pd2 137.88(5) . . ?
O1 Pd1 Pd2 74.12(4) . . ?
C25 Pd2 N2 95.77(8) . . ?
C25 Pd2 N3 82.84(8) . . ?
N2 Pd2 N3 177.33(7) . . ?
C25 Pd2 O2 176.08(7) . . ?
N2 Pd2 O2 88.15(6) . . ?
N3 Pd2 O2 93.26(7) . . ?
C25 Pd2 Pd1 101.10(6) . . ?
N2 Pd2 Pd1 38.89(4) . . ?
N3 Pd2 Pd1 143.59(5) . . ?
O2 Pd2 Pd1 81.85(4) . . ?
C2 C1 C6 117.7(2) . . ?
C2 C1 Pd1 128.61(16) . . ?
C6 C1 Pd1 113.63(16) . . ?
C3 C2 C1 121.2(2) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C4 C3 C2 119.9(2) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.2(2) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.1(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.8(2) . . ?
C5 C6 C7 122.1(2) . . ?
C1 C6 C7 117.04(19) . . ?
N1 C7 C6 109.17(17) . . ?
N1 C7 H7A 109.8 . . ?
C6 C7 H7A 109.8 . . ?
N1 C7 H7B 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
C9 N1 C8 108.66(18) . . ?
C9 N1 C7 110.46(18) . . ?
C8 N1 C7 109.45(17) . . ?
C9 N1 Pd1 106.47(13) . . ?
C8 N1 Pd1 114.35(13) . . ?
C7 N1 Pd1 107.39(12) . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 N2 Pd1 130.01(14) . . ?
C10 N2 Pd2 123.64(14) . . ?
Pd1 N2 Pd2 102.04(7) . . ?
N2 C10 C11 122.34(18) . . ?
N2 C10 C17 121.67(18) . . ?
C11 C10 C17 115.87(17) . . ?
C16 C11 C12 119.1(2) . . ?
C16 C11 C10 119.5(2) . . ?
C12 C11 C10 121.5(2) . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C14 C13 C12 120.7(3) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 119.7(2) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C11 120.2(3) . . ?
C15 C16 H16 119.9 . . ?
C11 C16 H16 119.9 . . ?
C18 C17 C22 118.6(2) . . ?
C18 C17 C10 117.91(19) . . ?
C22 C17 C10 123.36(19) . . ?
C19 C18 C17 120.9(2) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 C18 120.2(2) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 119.7(2) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C20 C21 C22 120.4(2) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C21 C22 C17 120.2(2) . . ?
C21 C22 H22 119.9 . . ?
C17 C22 H22 119.9 . . ?
C23 O1 Pd1 130.94(14) . . ?
C23 O2 Pd2 122.57(14) . . ?
O1 C23 O2 126.8(2) . . ?
O1 C23 C24 115.7(2) . . ?
O2 C23 C24 117.6(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 116.9(2) . . ?
C26 C25 Pd2 128.68(16) . . ?
C30 C25 Pd2 114.40(16) . . ?
C27 C26 C25 121.8(2) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C28 C27 C26 120.3(2) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C29 C28 C27 119.5(2) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 120.3(2) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C25 121.1(2) . . ?
C29 C30 C31 122.5(2) . . ?
C25 C30 C31 116.3(2) . . ?
N3 C31 C30 109.99(18) . . ?
N3 C31 H31A 109.7 . . ?
C30 C31 H31A 109.7 . . ?
N3 C31 H31B 109.7 . . ?
C30 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C32 N3 C33 109.52(19) . . ?
C32 N3 C31 109.34(18) . . ?
C33 N3 C31 109.80(19) . . ?
C32 N3 Pd2 112.99(14) . . ?
C33 N3 Pd2 106.60(14) . . ?
C31 N3 Pd2 108.52(13) . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C36 119.4(4) 2_565 . ?
C35 C34 H34 120.3 2_565 . ?
C36 C34 H34 120.3 . . ?
C34 C35 C36 119.7(4) 2_565 . ?
C34 C35 H35 120.1 2_565 . ?
C36 C35 H35 120.1 . . ?
C35 C36 C34 120.8(4) . . ?
C35 C36 H36 119.6 . . ?
C34 C36 H36 119.6 . . ?
C42 C41 C46 120.0 . . ?
C42 C41 H41 120.0 . . ?
C46 C41 H41 120.0 . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C44 C43 C42 120.0 . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C45 C44 C43 120.0 . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
C46 C45 C44 120.0 . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C45 C46 C41 120.0 . . ?
C45 C46 H46 120.0 . . ?
C41 C46 H46 120.0 . . ?
C52 C51 C56 120.0 . . ?
C52 C51 H51 120.0 . . ?
C56 C51 H51 120.0 . . ?
C53 C52 C51 120.0 . . ?
C53 C52 H52 120.0 . . ?
C51 C52 H52 120.0 . . ?
C54 C53 C52 120.0 . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C55 C54 C53 120.0 . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
C54 C55 C56 120.0 . . ?
C54 C55 H55 120.0 . . ?
C56 C55 H55 120.0 . . ?
C55 C56 C51 120.0 . . ?
C55 C56 H56 120.0 . . ?
C51 C56 H56 120.0 . . ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full 26.35
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max 0.360
_refine_diff_density_min -0.408
_refine_diff_density_rms 0.056
# Attachment '1-1.5toluene.CIF'
data_vrr171cs
_database_code_depnum_ccdc_archive 'CCDC 694834'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Bis{(N,N-dimethylbenzylamine-\kN,\kC)palladium(II)}(\m-acetato-\kO:\kO')
(\m-benzophenone iminato-\kN:\kN) . 1.5toluene
;
_chemical_name_common
;
Bis((N,N-dimethylbenzylamine-kappaN,kappaC)palladium(ii))(mu-
acetato-kappaO:kappaO') (mu-benzophenone iminato-kappaN:kappaN) .
1.5toluene
;
_chemical_melting_point ?
_chemical_formula_moiety 'C33 H37 N3 O2 Pd2, 1.5(C7 H8)'
_chemical_formula_sum 'C43.50 H49 N3 O2 Pd2'
_chemical_formula_weight 858.66
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'
Pd Pd -0.9988 1.0072 '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_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.5075(5)
_cell_length_b 11.3472(6)
_cell_length_c 18.5747(10)
_cell_angle_alpha 82.7420(10)
_cell_angle_beta 83.1070(10)
_cell_angle_gamma 75.9870(10)
_cell_volume 1920.35(18)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9999
_cell_measurement_theta_min 2.2
_cell_measurement_theta_max 27.95
_exptl_crystal_description isometric
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.485
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 878
_exptl_absorpt_coefficient_mu 0.976
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8439
_exptl_absorpt_correction_T_max 0.9260
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(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 CCD area diffractometer'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 21096
_diffrn_reflns_av_R_equivalents 0.0218
_diffrn_reflns_av_sigmaI/netI 0.0273
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 1.86
_diffrn_reflns_theta_max 26.35
_reflns_number_total 7772
_reflns_number_gt 7089
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker 1997)'
_computing_cell_refinement SMART
_computing_data_reduction 'SAINT (Bruker 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2006)'
_computing_publication_material ?
_publ_section_references
;
Bruker (1997). Smart and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2006). DIAMOND. Version3.1e. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
One toluene is fully ordered. The other toluene is half-occupied around
the inversion center and was refined using the PART -1 command. For this
inversion disordered toluene the carbon atoms were refined isotropically,
its hydrogen atoms could be calculated. Hydrogen atoms on the methyl groups
C24, C34 and C41
were positioned with a rotating group refinement (AFIX 137).
;
_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^)+(0.0349P)^2^+2.3412P] 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 7772
_refine_ls_number_parameters 455
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0365
_refine_ls_R_factor_gt 0.0324
_refine_ls_wR_factor_ref 0.0766
_refine_ls_wR_factor_gt 0.0746
_refine_ls_goodness_of_fit_ref 1.086
_refine_ls_restrained_S_all 1.086
_refine_ls_shift/su_max 0.003
_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 0.52066(2) 0.727009(17) 0.693189(11) 0.01493(6) Uani 1 1 d . . .
Pd2 Pd 0.60890(2) 0.456128(17) 0.656377(11) 0.01510(6) Uani 1 1 d . . .
C1 C 0.3296(3) 0.7861(2) 0.65314(14) 0.0170(5) Uani 1 1 d . . .
C2 C 0.2129(3) 0.7294(2) 0.66093(15) 0.0193(6) Uani 1 1 d . . .
H2 H 0.2211 0.6521 0.6886 0.023 Uiso 1 1 calc R . .
C3 C 0.0848(3) 0.7839(3) 0.62894(15) 0.0213(6) Uani 1 1 d . . .
H3 H 0.0070 0.7435 0.6347 0.026 Uiso 1 1 calc R . .
C4 C 0.0701(3) 0.8972(3) 0.58859(16) 0.0241(6) Uani 1 1 d . . .
H4 H -0.0176 0.9342 0.5669 0.029 Uiso 1 1 calc R . .
C5 C 0.1835(3) 0.9559(3) 0.58000(16) 0.0230(6) Uani 1 1 d . . .
H5 H 0.1734 1.0337 0.5527 0.028 Uiso 1 1 calc R . .
C6 C 0.3134(3) 0.9006(2) 0.61151(15) 0.0188(6) Uani 1 1 d . . .
C7 C 0.4429(3) 0.9553(3) 0.59849(16) 0.0227(6) Uani 1 1 d . . .
H7A H 0.4112 1.0452 0.5977 0.027 Uiso 1 1 calc R . .
H7B H 0.4958 0.9359 0.5506 0.027 Uiso 1 1 calc R . .
N1 N 0.5413(2) 0.9057(2) 0.65749(13) 0.0198(5) Uani 1 1 d . . .
C8 C 0.6912(3) 0.9149(3) 0.63062(18) 0.0276(7) Uani 1 1 d . . .
H8A H 0.7556 0.8824 0.6695 0.041 Uiso 1 1 calc R . .
H8B H 0.6928 1.0006 0.6159 0.041 Uiso 1 1 calc R . .
H8C H 0.7248 0.8676 0.5886 0.041 Uiso 1 1 calc R . .
C9 C 0.4899(3) 0.9784(3) 0.72083(17) 0.0272(7) Uani 1 1 d . . .
H9A H 0.3900 0.9731 0.7384 0.041 Uiso 1 1 calc R . .
H9B H 0.4923 1.0640 0.7058 0.041 Uiso 1 1 calc R . .
H9C H 0.5536 0.9462 0.7600 0.041 Uiso 1 1 calc R . .
N2 N 0.4908(2) 0.5606(2) 0.73063(12) 0.0159(5) Uani 1 1 d . . .
C10 C 0.4475(3) 0.5321(2) 0.79697(15) 0.0173(5) Uani 1 1 d . . .
C11 C 0.4114(3) 0.6243(2) 0.85193(15) 0.0200(6) Uani 1 1 d . . .
C12 C 0.4904(4) 0.5998(3) 0.91227(18) 0.0359(8) Uani 1 1 d . . .
H12 H 0.5551 0.5222 0.9205 0.043 Uiso 1 1 calc R . .
C13 C 0.4776(4) 0.6853(3) 0.9608(2) 0.0420(9) Uani 1 1 d . . .
H13 H 0.5359 0.6675 1.0007 0.050 Uiso 1 1 calc R . .
C14 C 0.3803(4) 0.7965(3) 0.95133(18) 0.0368(8) Uani 1 1 d . . .
H14 H 0.3717 0.8561 0.9842 0.044 Uiso 1 1 calc R . .
C15 C 0.2954(4) 0.8205(3) 0.89338(18) 0.0381(9) Uani 1 1 d . . .
H15 H 0.2251 0.8956 0.8877 0.046 Uiso 1 1 calc R . .
C16 C 0.3118(4) 0.7360(3) 0.84348(16) 0.0303(7) Uani 1 1 d . . .
H16 H 0.2546 0.7545 0.8032 0.036 Uiso 1 1 calc R . .
C17 C 0.4425(3) 0.4042(2) 0.82675(14) 0.0193(6) Uani 1 1 d . . .
C18 C 0.5600(3) 0.3059(3) 0.81422(15) 0.0212(6) Uani 1 1 d . . .
H18 H 0.6468 0.3197 0.7871 0.025 Uiso 1 1 calc R . .
C19 C 0.5508(3) 0.1884(3) 0.84105(16) 0.0272(7) Uani 1 1 d . . .
H19 H 0.6318 0.1221 0.8327 0.033 Uiso 1 1 calc R . .
C20 C 0.4243(4) 0.1667(3) 0.88002(17) 0.0302(7) Uani 1 1 d . . .
H20 H 0.4177 0.0856 0.8974 0.036 Uiso 1 1 calc R . .
C21 C 0.3074(4) 0.2638(3) 0.89351(17) 0.0294(7) Uani 1 1 d . . .
H21 H 0.2205 0.2493 0.9202 0.035 Uiso 1 1 calc R . .
C22 C 0.3172(3) 0.3820(3) 0.86816(15) 0.0232(6) Uani 1 1 d . . .
H22 H 0.2381 0.4484 0.8790 0.028 Uiso 1 1 calc R . .
O1 O 0.7311(2) 0.67628(17) 0.73254(11) 0.0221(4) Uani 1 1 d . . .
O2 O 0.8005(2) 0.49038(18) 0.69195(11) 0.0238(4) Uani 1 1 d . . .
C23 C 0.8194(3) 0.5752(3) 0.72430(15) 0.0196(6) Uani 1 1 d . . .
C24 C 0.9641(3) 0.5524(3) 0.75538(18) 0.0290(7) Uani 1 1 d . . .
H24A H 1.0429 0.5311 0.7168 0.043 Uiso 1 1 calc R . .
H24B H 0.9710 0.4849 0.7943 0.043 Uiso 1 1 calc R . .
H24C H 0.9723 0.6262 0.7752 0.043 Uiso 1 1 calc R . .
C25 C 0.4553(3) 0.3904(2) 0.62457(15) 0.0177(5) Uani 1 1 d . . .
C26 C 0.3194(3) 0.3840(3) 0.66078(15) 0.0208(6) Uani 1 1 d . . .
H26 H 0.2919 0.4139 0.7071 0.025 Uiso 1 1 calc R . .
C27 C 0.2235(3) 0.3340(3) 0.62970(17) 0.0241(6) Uani 1 1 d . . .
H27 H 0.1317 0.3300 0.6552 0.029 Uiso 1 1 calc R . .
C28 C 0.2610(3) 0.2903(3) 0.56197(18) 0.0258(6) Uani 1 1 d . . .
H28 H 0.1942 0.2585 0.5405 0.031 Uiso 1 1 calc R . .
C29 C 0.3959(3) 0.2931(3) 0.52587(17) 0.0246(6) Uani 1 1 d . . .
H29 H 0.4224 0.2626 0.4796 0.030 Uiso 1 1 calc R . .
C30 C 0.4935(3) 0.3408(2) 0.55719(15) 0.0197(6) Uani 1 1 d . . .
C31 C 0.6408(3) 0.3476(3) 0.51974(15) 0.0220(6) Uani 1 1 d . . .
H31A H 0.6828 0.2739 0.4941 0.026 Uiso 1 1 calc R . .
H31B H 0.6317 0.4200 0.4833 0.026 Uiso 1 1 calc R . .
N3 N 0.7380(2) 0.3564(2) 0.57533(12) 0.0187(5) Uani 1 1 d . . .
C32 C 0.8595(3) 0.4095(3) 0.53928(17) 0.0262(6) Uani 1 1 d . . .
H32A H 0.8203 0.4912 0.5156 0.039 Uiso 1 1 calc R . .
H32B H 0.9152 0.3572 0.5026 0.039 Uiso 1 1 calc R . .
H32C H 0.9233 0.4151 0.5758 0.039 Uiso 1 1 calc R . .
C33 C 0.7994(3) 0.2329(3) 0.61079(17) 0.0247(6) Uani 1 1 d . . .
H33A H 0.7200 0.1969 0.6351 0.037 Uiso 1 1 calc R . .
H33B H 0.8638 0.2391 0.6469 0.037 Uiso 1 1 calc R . .
H33C H 0.8549 0.1810 0.5738 0.037 Uiso 1 1 calc R . .
C34 C 1.0496(5) 1.1380(5) 0.7844(3) 0.0762(15) Uani 1 1 d . . .
H34A H 1.1283 1.1431 0.8126 0.114 Uiso 1 1 calc R . .
H34B H 0.9846 1.2190 0.7765 0.114 Uiso 1 1 calc R . .
H34C H 1.0910 1.1088 0.7372 0.114 Uiso 1 1 calc R . .
C35 C 0.9657(4) 1.0516(4) 0.8252(2) 0.0471(10) Uani 1 1 d . . .
C36 C 0.9262(4) 0.9656(4) 0.7901(2) 0.0458(10) Uani 1 1 d . . .
H36 H 0.9559 0.9600 0.7397 0.055 Uiso 1 1 calc R . .
C37 C 0.8442(5) 0.8878(3) 0.8270(2) 0.0534(12) Uani 1 1 d . . .
H37 H 0.8162 0.8310 0.8015 0.064 Uiso 1 1 calc R . .
C38 C 0.8022(5) 0.8920(4) 0.9010(3) 0.0551(11) Uani 1 1 d . . .
H38 H 0.7446 0.8392 0.9262 0.066 Uiso 1 1 calc R . .
C39 C 0.8451(5) 0.9732(4) 0.9369(2) 0.0521(11) Uani 1 1 d . . .
H39 H 0.8206 0.9746 0.9880 0.063 Uiso 1 1 calc R . .
C40 C 0.9232(4) 1.0529(4) 0.9001(2) 0.0481(10) Uani 1 1 d . . .
H40 H 0.9490 1.1104 0.9260 0.058 Uiso 1 1 calc R . .
C41 C 0.8464(14) 0.4044(12) 0.9398(8) 0.085(4) Uiso 0.50 1 d P A -1
H41A H 0.7824 0.3684 0.9768 0.128 Uiso 0.50 1 calc PR A -1
H41B H 0.9084 0.3404 0.9118 0.128 Uiso 0.50 1 calc PR A -1
H41C H 0.7872 0.4659 0.9069 0.128 Uiso 0.50 1 calc PR A -1
C42 C 0.9424(10) 0.4652(8) 0.9771(5) 0.053(2) Uiso 0.50 1 d P A -1
C43 C 0.9460(7) 0.5794(6) 0.9502(4) 0.0215(13) Uiso 0.50 1 d P A -1
H43 H 0.8876 0.6211 0.9126 0.026 Uiso 0.50 1 calc PR A -1
C44 C 1.0460(9) 0.6398(8) 0.9817(4) 0.0472(19) Uiso 0.50 1 d P A -1
H44 H 1.0471 0.7224 0.9654 0.057 Uiso 0.50 1 calc PR A -1
C45 C 1.1332(10) 0.5796(8) 1.0321(5) 0.047(2) Uiso 0.50 1 d P A -1
H45 H 1.2026 0.6153 1.0486 0.056 Uiso 0.50 1 calc PR A -1
C46 C 1.1189(12) 0.4599(10) 1.0605(6) 0.069(3) Uiso 0.50 1 d P A -1
H46 H 1.1731 0.4183 1.0997 0.083 Uiso 0.50 1 calc PR A -1
C47 C 1.0208(9) 0.3994(7) 1.0300(4) 0.0361(17) Uiso 0.50 1 d P A -1
H47 H 1.0138 0.3182 1.0469 0.043 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 0.01556(11) 0.01299(11) 0.01546(11) -0.00117(8) -0.00190(8) -0.00168(8)
Pd2 0.01553(11) 0.01323(11) 0.01559(11) -0.00173(8) -0.00067(8) -0.00174(8)
C1 0.0182(13) 0.0164(13) 0.0148(13) -0.0034(10) 0.0002(10) -0.0005(10)
C2 0.0226(14) 0.0165(13) 0.0168(13) -0.0005(10) -0.0006(11) -0.0018(11)
C3 0.0202(14) 0.0236(15) 0.0192(14) -0.0022(11) -0.0023(11) -0.0031(11)
C4 0.0224(15) 0.0257(15) 0.0211(14) -0.0013(12) -0.0055(11) 0.0013(12)
C5 0.0286(15) 0.0169(14) 0.0211(14) 0.0008(11) -0.0033(12) -0.0013(12)
C6 0.0208(14) 0.0175(13) 0.0176(13) -0.0030(10) -0.0015(11) -0.0029(11)
C7 0.0271(15) 0.0152(14) 0.0241(15) 0.0026(11) -0.0047(12) -0.0029(11)
N1 0.0198(12) 0.0145(11) 0.0246(12) -0.0018(9) -0.0024(10) -0.0032(9)
C8 0.0222(15) 0.0225(15) 0.0383(18) -0.0023(13) 0.0008(13) -0.0079(12)
C9 0.0300(16) 0.0198(15) 0.0325(17) -0.0113(13) -0.0037(13) -0.0021(12)
N2 0.0148(11) 0.0137(11) 0.0176(11) -0.0010(9) -0.0028(9) 0.0000(9)
C10 0.0142(13) 0.0164(13) 0.0193(14) -0.0001(10) -0.0040(10) 0.0005(10)
C11 0.0227(14) 0.0178(14) 0.0175(14) -0.0004(11) 0.0008(11) -0.0026(11)
C12 0.048(2) 0.0231(16) 0.0332(18) -0.0065(13) -0.0192(16) 0.0076(14)
C13 0.058(2) 0.0339(19) 0.0326(19) -0.0091(15) -0.0209(17) 0.0031(17)
C14 0.057(2) 0.0262(17) 0.0241(16) -0.0102(13) -0.0016(15) -0.0012(15)
C15 0.051(2) 0.0251(17) 0.0268(17) -0.0075(13) -0.0043(15) 0.0158(15)
C16 0.0358(18) 0.0281(16) 0.0184(15) -0.0028(12) -0.0056(13) 0.0107(13)
C17 0.0241(14) 0.0184(14) 0.0143(13) -0.0002(10) -0.0058(11) -0.0019(11)
C18 0.0234(14) 0.0199(14) 0.0182(14) -0.0005(11) -0.0043(11) -0.0007(11)
C19 0.0345(17) 0.0195(15) 0.0241(15) -0.0030(12) -0.0076(13) 0.0031(13)
C20 0.046(2) 0.0195(15) 0.0266(16) 0.0038(12) -0.0075(14) -0.0121(14)
C21 0.0325(17) 0.0339(18) 0.0235(16) 0.0015(13) 0.0002(13) -0.0142(14)
C22 0.0235(15) 0.0256(15) 0.0187(14) 0.0004(11) -0.0013(11) -0.0041(12)
O1 0.0195(10) 0.0181(10) 0.0289(11) -0.0041(8) -0.0057(8) -0.0019(8)
O2 0.0186(10) 0.0236(11) 0.0291(11) -0.0086(9) -0.0015(8) -0.0021(8)
C23 0.0200(14) 0.0199(14) 0.0181(14) -0.0002(11) 0.0015(11) -0.0054(11)
C24 0.0235(15) 0.0230(16) 0.0399(19) -0.0027(13) -0.0085(13) -0.0019(12)
C25 0.0210(14) 0.0109(12) 0.0206(14) 0.0010(10) -0.0063(11) -0.0019(10)
C26 0.0214(14) 0.0193(14) 0.0201(14) -0.0011(11) -0.0020(11) -0.0021(11)
C27 0.0184(14) 0.0193(14) 0.0333(17) 0.0016(12) -0.0050(12) -0.0028(11)
C28 0.0249(15) 0.0160(14) 0.0382(18) -0.0044(12) -0.0143(13) -0.0016(12)
C29 0.0268(15) 0.0176(14) 0.0288(16) -0.0075(12) -0.0093(12) 0.0020(12)
C30 0.0204(14) 0.0132(13) 0.0225(14) -0.0007(11) -0.0044(11) 0.0023(10)
C31 0.0252(15) 0.0213(14) 0.0180(14) -0.0054(11) -0.0032(11) -0.0004(11)
N3 0.0188(11) 0.0152(11) 0.0197(12) -0.0005(9) -0.0021(9) -0.0003(9)
C32 0.0204(14) 0.0290(16) 0.0273(16) -0.0055(13) 0.0032(12) -0.0034(12)
C33 0.0270(15) 0.0164(14) 0.0271(16) -0.0013(12) -0.0050(12) 0.0029(12)
C34 0.046(3) 0.102(4) 0.085(4) 0.002(3) -0.019(3) -0.025(3)
C35 0.0308(19) 0.061(3) 0.045(2) -0.0106(19) -0.0148(16) 0.0047(17)
C36 0.046(2) 0.051(2) 0.0318(19) -0.0168(17) -0.0134(16) 0.0159(18)
C37 0.070(3) 0.029(2) 0.057(3) -0.0130(18) -0.033(2) 0.0154(19)
C38 0.058(3) 0.035(2) 0.061(3) 0.0065(19) -0.017(2) 0.0110(19)
C39 0.058(3) 0.048(2) 0.036(2) -0.0050(18) -0.0088(19) 0.017(2)
C40 0.051(2) 0.050(2) 0.041(2) -0.0227(19) -0.0215(18) 0.0102(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 C1 1.978(3) . ?
Pd1 N2 2.002(2) . ?
Pd1 N1 2.100(2) . ?
Pd1 O1 2.1342(19) . ?
Pd1 Pd2 3.1247(3) . ?
Pd2 C25 1.970(3) . ?
Pd2 N2 1.991(2) . ?
Pd2 N3 2.090(2) . ?
Pd2 O2 2.145(2) . ?
C1 C2 1.396(4) . ?
C1 C6 1.410(4) . ?
C2 C3 1.391(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.403(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.490(4) . ?
C7 N1 1.493(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N1 C8 1.476(4) . ?
N1 C9 1.489(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N2 C10 1.279(3) . ?
C10 C17 1.496(4) . ?
C10 C11 1.505(4) . ?
C11 C12 1.386(4) . ?
C11 C16 1.390(4) . ?
C12 C13 1.381(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.377(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.395(4) . ?
C17 C22 1.397(4) . ?
C18 C19 1.382(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.386(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.386(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.385(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
O1 C23 1.261(3) . ?
O2 C23 1.255(3) . ?
C23 C24 1.508(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.398(4) . ?
C25 C30 1.409(4) . ?
C26 C27 1.395(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.386(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.394(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.502(4) . ?
C31 N3 1.493(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
N3 C32 1.481(4) . ?
N3 C33 1.484(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.489(7) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.383(6) . ?
C35 C40 1.403(6) . ?
C36 C37 1.382(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.387(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.365(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.373(6) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C42 1.539(15) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.336(11) . ?
C42 C47 1.340(12) . ?
C43 C44 1.505(10) . ?
C43 H43 0.9500 . ?
C44 C45 1.335(12) . ?
C44 H44 0.9500 . ?
C45 C46 1.425(14) . ?
C45 H45 0.9500 . ?
C46 C47 1.484(13) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
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
C1 Pd1 N2 95.42(10) . . ?
C1 Pd1 N1 82.85(10) . . ?
N2 Pd1 N1 176.80(9) . . ?
C1 Pd1 O1 175.49(9) . . ?
N2 Pd1 O1 89.06(8) . . ?
N1 Pd1 O1 92.70(8) . . ?
C1 Pd1 Pd2 101.99(8) . . ?
N2 Pd1 Pd2 38.39(6) . . ?
N1 Pd1 Pd2 144.59(6) . . ?
O1 Pd1 Pd2 81.23(5) . . ?
C25 Pd2 N2 99.63(10) . . ?
C25 Pd2 N3 82.71(10) . . ?
N2 Pd2 N3 176.23(9) . . ?
C25 Pd2 O2 168.51(9) . . ?
N2 Pd2 O2 88.34(8) . . ?
N3 Pd2 O2 89.78(8) . . ?
C25 Pd2 Pd1 116.63(8) . . ?
N2 Pd2 Pd1 38.64(6) . . ?
N3 Pd2 Pd1 137.62(6) . . ?
O2 Pd2 Pd1 74.71(5) . . ?
C2 C1 C6 117.7(2) . . ?
C2 C1 Pd1 128.5(2) . . ?
C6 C1 Pd1 113.8(2) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C4 C3 C2 120.3(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C4 C3 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.8(3) . . ?
C5 C6 C7 121.9(3) . . ?
C1 C6 C7 117.1(2) . . ?
C6 C7 N1 109.6(2) . . ?
C6 C7 H7A 109.7 . . ?
N1 C7 H7A 109.7 . . ?
C6 C7 H7B 109.7 . . ?
N1 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C8 N1 C9 109.4(2) . . ?
C8 N1 C7 109.6(2) . . ?
C9 N1 C7 108.9(2) . . ?
C8 N1 Pd1 114.07(17) . . ?
C9 N1 Pd1 106.65(18) . . ?
C7 N1 Pd1 108.09(17) . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 N2 Pd2 130.15(19) . . ?
C10 N2 Pd1 123.08(19) . . ?
Pd2 N2 Pd1 102.96(10) . . ?
N2 C10 C17 122.8(2) . . ?
N2 C10 C11 121.4(2) . . ?
C17 C10 C11 115.5(2) . . ?
C12 C11 C16 117.9(3) . . ?
C12 C11 C10 117.6(3) . . ?
C16 C11 C10 124.3(3) . . ?
C13 C12 C11 121.7(3) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 119.3(3) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C11 120.5(3) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C18 C17 C22 118.8(3) . . ?
C18 C17 C10 121.7(3) . . ?
C22 C17 C10 119.4(2) . . ?
C19 C18 C17 120.4(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 120.4(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C21 119.7(3) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 120.1(3) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C17 120.5(3) . . ?
C21 C22 H22 119.7 . . ?
C17 C22 H22 119.7 . . ?
C23 O1 Pd1 123.80(18) . . ?
C23 O2 Pd2 131.81(18) . . ?
O2 C23 O1 126.8(3) . . ?
O2 C23 C24 115.6(2) . . ?
O1 C23 C24 117.7(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 117.6(3) . . ?
C26 C25 Pd2 128.7(2) . . ?
C30 C25 Pd2 113.7(2) . . ?
C27 C26 C25 120.8(3) . . ?
C27 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C28 C27 C26 120.5(3) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.1(3) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 121.2(3) . . ?
C29 C30 C31 122.2(3) . . ?
C25 C30 C31 116.6(2) . . ?
N3 C31 C30 109.1(2) . . ?
N3 C31 H31A 109.9 . . ?
C30 C31 H31A 109.9 . . ?
N3 C31 H31B 109.9 . . ?
C30 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
C32 N3 C33 108.7(2) . . ?
C32 N3 C31 109.5(2) . . ?
C33 N3 C31 109.8(2) . . ?
C32 N3 Pd2 114.44(17) . . ?
C33 N3 Pd2 106.84(17) . . ?
C31 N3 Pd2 107.49(16) . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C40 116.9(4) . . ?
C36 C35 C34 120.8(4) . . ?
C40 C35 C34 122.2(4) . . ?
C37 C36 C35 121.2(4) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C36 C37 C38 120.7(4) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C39 C38 C37 118.8(5) . . ?
C39 C38 H38 120.6 . . ?
C37 C38 H38 120.6 . . ?
C38 C39 C40 120.8(4) . . ?
C38 C39 H39 119.6 . . ?
C40 C39 H39 119.6 . . ?
C39 C40 C35 121.6(4) . . ?
C39 C40 H40 119.2 . . ?
C35 C40 H40 119.2 . . ?
C43 C42 C47 125.4(8) . . ?
C43 C42 C41 115.6(9) . . ?
C47 C42 C41 118.9(10) . . ?
C42 C43 C44 117.6(7) . . ?
C42 C43 H43 121.2 . . ?
C44 C43 H43 121.2 . . ?
C45 C44 C43 121.3(8) . . ?
C45 C44 H44 119.4 . . ?
C43 C44 H44 119.4 . . ?
C44 C45 C46 117.9(10) . . ?
C44 C45 H45 121.0 . . ?
C46 C45 H45 121.0 . . ?
C45 C46 C47 121.1(10) . . ?
C45 C46 H46 119.5 . . ?
C47 C46 H46 119.5 . . ?
C42 C47 C46 116.5(8) . . ?
C42 C47 H47 121.8 . . ?
C46 C47 H47 121.8 . . ?
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 26.35
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 0.952
_refine_diff_density_min -0.493
_refine_diff_density_rms 0.090
# Attachment '1-hexane.cif'
data_vrr171bs
_database_code_depnum_ccdc_archive 'CCDC 694835'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
[\m-Acetato-\m-benzophenone iminato-
bis{N,N-dimethylbenzylamine-\kN,\kC-palladium(II)}] 1(n-hexane)
;
_chemical_name_common '[{(dmba)Pd}2(m-OAc)(m-N=CPh2)].1(n-hexane)'
_chemical_melting_point ?
_chemical_formula_moiety 'C33 H37 N3 O2 Pd2, C6 H14'
_chemical_formula_sum 'C39 H51 N3 O2 Pd2'
_chemical_formula_weight 806.63
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/c
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 14.2859(6)
_cell_length_b 28.3485(12)
_cell_length_c 9.2862(4)
_cell_angle_alpha 90.00
_cell_angle_beta 103.8940(10)
_cell_angle_gamma 90.00
_cell_volume 3650.7(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9999
_cell_measurement_theta_min 2.37
_cell_measurement_theta_max 28.065
_exptl_crystal_description isometric
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.11
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.468
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1656
_exptl_absorpt_coefficient_mu 1.022
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.7843
_exptl_absorpt_correction_T_max 0.8959
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(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 diffractometer'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 39888
_diffrn_reflns_av_R_equivalents 0.0230
_diffrn_reflns_av_sigmaI/netI 0.0172
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -35
_diffrn_reflns_limit_k_max 35
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_theta_min 1.63
_diffrn_reflns_theta_max 26.40
_reflns_number_total 7491
_reflns_number_gt 7157
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker, 1997)'
_computing_cell_refinement 'SAINT (Bruker, 1997)'
_computing_data_reduction 'SAINT (Bruker 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2006)'
_computing_publication_material ?
_publ_section_references
;
Bruker (1997). SMART and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2006). DIAMOND. Version 3.1e. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
For the most part the n-hexane molecule is disordered over more than
two positions. For the central section of the molecule two major position
were found, one with about 0.7 occupancy (PART 1), the other with about
0.3 occupancy (PART 2). At one end of the n-hexane chain additional
positions were found. The carbon atoms could be refined isotropically only,
yet their their hydrogen atoms could still be calculated.
In total there is one n-hexane molecule per asymmetric unit.
;
_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^)+(0.0316P)^2^+4.8199P] 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 7491
_refine_ls_number_parameters 422
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0312
_refine_ls_R_factor_gt 0.0296
_refine_ls_wR_factor_ref 0.0725
_refine_ls_wR_factor_gt 0.0717
_refine_ls_goodness_of_fit_ref 1.135
_refine_ls_restrained_S_all 1.135
_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 0.205602(13) 0.460808(6) 0.97068(2) 0.01762(6) Uani 1 1 d . . .
Pd2 Pd 0.158493(13) 0.356359(6) 0.99120(2) 0.01736(6) Uani 1 1 d . . .
C1 C 0.18131(18) 0.50127(8) 1.1308(3) 0.0193(5) Uani 1 1 d . . .
C2 C 0.22191(18) 0.49810(9) 1.2834(3) 0.0223(5) Uani 1 1 d . . .
H2 H 0.2657 0.4733 1.3209 0.027 Uiso 1 1 calc R . .
C3 C 0.19882(19) 0.53091(10) 1.3807(3) 0.0257(5) Uani 1 1 d . . .
H3 H 0.2275 0.5285 1.4839 0.031 Uiso 1 1 calc R . .
C4 C 0.1344(2) 0.56697(10) 1.3285(3) 0.0308(6) Uani 1 1 d . . .
H4 H 0.1177 0.5887 1.3960 0.037 Uiso 1 1 calc R . .
C5 C 0.0941(2) 0.57132(9) 1.1771(3) 0.0275(6) Uani 1 1 d . . .
H5 H 0.0504 0.5962 1.1407 0.033 Uiso 1 1 calc R . .
C6 C 0.11835(19) 0.53885(9) 1.0790(3) 0.0224(5) Uani 1 1 d . . .
C7 C 0.07603(19) 0.54140(9) 0.9153(3) 0.0241(5) Uani 1 1 d . . .
H7A H 0.0120 0.5259 0.8904 0.029 Uiso 1 1 calc R . .
H7B H 0.0676 0.5748 0.8834 0.029 Uiso 1 1 calc R . .
N1 N 0.14246(15) 0.51711(7) 0.8372(2) 0.0209(4) Uani 1 1 d . . .
C8 C 0.0887(2) 0.50268(10) 0.6871(3) 0.0289(6) Uani 1 1 d . . .
H8A H 0.0364 0.4812 0.6950 0.043 Uiso 1 1 calc R . .
H8B H 0.1325 0.4867 0.6364 0.043 Uiso 1 1 calc R . .
H8C H 0.0614 0.5307 0.6302 0.043 Uiso 1 1 calc R . .
C9 C 0.2210(2) 0.54962(10) 0.8236(3) 0.0282(6) Uani 1 1 d . . .
H9A H 0.2570 0.5594 0.9226 0.042 Uiso 1 1 calc R . .
H9B H 0.1934 0.5775 0.7663 0.042 Uiso 1 1 calc R . .
H9C H 0.2646 0.5335 0.7728 0.042 Uiso 1 1 calc R . .
N2 N 0.25661(14) 0.40379(7) 1.0895(2) 0.0189(4) Uani 1 1 d . . .
C10 C 0.34027(18) 0.39261(9) 1.1657(3) 0.0198(5) Uani 1 1 d . . .
C11 C 0.41844(18) 0.42768(9) 1.2244(3) 0.0220(5) Uani 1 1 d . . .
C12 C 0.4319(2) 0.46792(10) 1.1447(3) 0.0285(6) Uani 1 1 d . . .
H12 H 0.3904 0.4737 1.0498 0.034 Uiso 1 1 calc R . .
C13 C 0.5054(2) 0.49951(10) 1.2029(4) 0.0331(6) Uani 1 1 d . . .
H13 H 0.5144 0.5265 1.1471 0.040 Uiso 1 1 calc R . .
C14 C 0.5656(2) 0.49204(11) 1.3415(3) 0.0334(6) Uani 1 1 d . . .
H14 H 0.6154 0.5140 1.3813 0.040 Uiso 1 1 calc R . .
C15 C 0.5530(2) 0.45252(11) 1.4217(3) 0.0342(6) Uani 1 1 d . . .
H15 H 0.5940 0.4474 1.5174 0.041 Uiso 1 1 calc R . .
C16 C 0.48109(19) 0.42043(10) 1.3633(3) 0.0275(6) Uani 1 1 d . . .
H16 H 0.4741 0.3930 1.4186 0.033 Uiso 1 1 calc R . .
C17 C 0.36956(19) 0.34170(9) 1.1951(3) 0.0246(5) Uani 1 1 d . . .
C18 C 0.4462(3) 0.32554(12) 1.1412(4) 0.0445(8) Uani 1 1 d . . .
H18 H 0.4799 0.3468 1.0927 0.053 Uiso 1 1 calc R . .
C19 C 0.4742(3) 0.27853(12) 1.1575(5) 0.0582(11) Uani 1 1 d . . .
H19 H 0.5257 0.2676 1.1179 0.070 Uiso 1 1 calc R . .
C20 C 0.4273(3) 0.24786(12) 1.2312(5) 0.0551(10) Uani 1 1 d . . .
H20 H 0.4467 0.2158 1.2433 0.066 Uiso 1 1 calc R . .
C21 C 0.3532(2) 0.26344(12) 1.2866(5) 0.0534(10) Uani 1 1 d . . .
H21 H 0.3215 0.2422 1.3384 0.064 Uiso 1 1 calc R . .
C22 C 0.3232(2) 0.31030(11) 1.2682(4) 0.0391(7) Uani 1 1 d . . .
H22 H 0.2705 0.3207 1.3061 0.047 Uiso 1 1 calc R . .
O1 O 0.24650(14) 0.42901(6) 0.7832(2) 0.0265(4) Uani 1 1 d . . .
O2 O 0.23010(14) 0.35109(6) 0.8161(2) 0.0256(4) Uani 1 1 d . . .
C23 C 0.25801(19) 0.38641(9) 0.7549(3) 0.0233(5) Uani 1 1 d . . .
C24 C 0.3109(2) 0.37624(10) 0.6350(3) 0.0322(6) Uani 1 1 d . . .
H24A H 0.3155 0.3421 0.6226 0.048 Uiso 1 1 calc R . .
H24B H 0.3759 0.3898 0.6637 0.048 Uiso 1 1 calc R . .
H24C H 0.2757 0.3903 0.5413 0.048 Uiso 1 1 calc R . .
C25 C 0.08538(18) 0.35520(8) 1.1466(3) 0.0193(5) Uani 1 1 d . . .
C26 C 0.10760(18) 0.37824(9) 1.2847(3) 0.0222(5) Uani 1 1 d . . .
H26 H 0.1645 0.3968 1.3118 0.027 Uiso 1 1 calc R . .
C27 C 0.0480(2) 0.37444(9) 1.3824(3) 0.0255(5) Uani 1 1 d . . .
H27 H 0.0649 0.3900 1.4756 0.031 Uiso 1 1 calc R . .
C28 C -0.0361(2) 0.34794(9) 1.3446(3) 0.0263(6) Uani 1 1 d . . .
H28 H -0.0771 0.3456 1.4111 0.032 Uiso 1 1 calc R . .
C29 C -0.05986(19) 0.32480(9) 1.2087(3) 0.0249(5) Uani 1 1 d . . .
H29 H -0.1174 0.3067 1.1822 0.030 Uiso 1 1 calc R . .
C30 C 0.00041(18) 0.32808(8) 1.1112(3) 0.0207(5) Uani 1 1 d . . .
C31 C -0.02583(19) 0.30576(9) 0.9602(3) 0.0230(5) Uani 1 1 d . . .
H31A H -0.0498 0.2733 0.9681 0.028 Uiso 1 1 calc R . .
H31B H -0.0780 0.3241 0.8946 0.028 Uiso 1 1 calc R . .
N3 N 0.05990(16) 0.30419(7) 0.8947(2) 0.0214(4) Uani 1 1 d . . .
C32 C 0.0290(2) 0.30715(10) 0.7318(3) 0.0294(6) Uani 1 1 d . . .
H32A H -0.0069 0.3365 0.7033 0.044 Uiso 1 1 calc R . .
H32B H -0.0124 0.2802 0.6935 0.044 Uiso 1 1 calc R . .
H32C H 0.0858 0.3067 0.6900 0.044 Uiso 1 1 calc R . .
C33 C 0.1144(2) 0.25960(9) 0.9376(3) 0.0290(6) Uani 1 1 d . . .
H33A H 0.1349 0.2576 1.0460 0.043 Uiso 1 1 calc R . .
H33B H 0.1713 0.2592 0.8959 0.043 Uiso 1 1 calc R . .
H33C H 0.0730 0.2326 0.8992 0.043 Uiso 1 1 calc R . .
C34 C 0.7024(5) 0.3342(3) 0.3494(8) 0.0665(17) Uiso 0.65 1 d P A 1
H34A H 0.6905 0.3220 0.2480 0.100 Uiso 0.65 1 calc PR A 1
H34B H 0.7584 0.3553 0.3683 0.100 Uiso 0.65 1 calc PR A 1
H34C H 0.6456 0.3517 0.3615 0.100 Uiso 0.65 1 calc PR A 1
C35 C 0.7227(6) 0.2918(3) 0.4630(8) 0.0743(18) Uiso 0.70 1 d P A 1
H35A H 0.6672 0.2699 0.4384 0.089 Uiso 0.70 1 calc PR A 1
H35B H 0.7800 0.2745 0.4489 0.089 Uiso 0.70 1 calc PR A 1
C36 C 0.7390(6) 0.3044(3) 0.6172(9) 0.074(2) Uiso 0.60 1 d P A 1
H36A H 0.8001 0.3224 0.6437 0.089 Uiso 0.60 1 calc PR A 1
H36B H 0.7497 0.2747 0.6751 0.089 Uiso 0.60 1 calc PR A 1
C37 C 0.6661(5) 0.3318(2) 0.6699(8) 0.0614(17) Uiso 0.70 1 d P A 1
H37A H 0.6060 0.3130 0.6461 0.074 Uiso 0.70 1 calc PR A 1
H37B H 0.6534 0.3606 0.6077 0.074 Uiso 0.70 1 calc PR A 1
C38 C 0.6810(6) 0.3482(3) 0.8338(9) 0.0626(18) Uiso 0.60 1 d P A 1
H38A H 0.7337 0.3717 0.8475 0.075 Uiso 0.60 1 calc PR A 1
H38B H 0.7091 0.3204 0.8932 0.075 Uiso 0.60 1 calc PR A 1
C39 C 0.6028(11) 0.3713(6) 0.9279(18) 0.066(4) Uiso 0.35 1 d P A 1
H39A H 0.6364 0.3762 1.0319 0.099 Uiso 0.35 1 calc PR A 1
H39B H 0.5490 0.3494 0.9224 0.099 Uiso 0.35 1 calc PR A 1
H39C H 0.5781 0.4015 0.8833 0.099 Uiso 0.35 1 calc PR A 1
C40 C 0.7211(11) 0.3000(6) 0.3415(18) 0.067(4) Uiso 0.30 1 d P B 2
H40A H 0.6879 0.2783 0.2637 0.101 Uiso 0.30 1 calc PR B 2
H40B H 0.7852 0.2875 0.3880 0.101 Uiso 0.30 1 calc PR B 2
H40C H 0.7276 0.3309 0.2976 0.101 Uiso 0.30 1 calc PR B 2
C41 C 0.6622(12) 0.3051(6) 0.4594(18) 0.069(4) Uiso 0.30 1 d P B 2
H41A H 0.5975 0.3169 0.4081 0.083 Uiso 0.30 1 calc PR B 2
H41B H 0.6529 0.2730 0.4957 0.083 Uiso 0.30 1 calc PR B 2
C42 C 0.6920(11) 0.3308(5) 0.5720(17) 0.061(3) Uiso 0.30 1 d P B 2
H42A H 0.7052 0.3620 0.5328 0.073 Uiso 0.30 1 calc PR B 2
H42B H 0.7556 0.3177 0.6228 0.073 Uiso 0.30 1 calc PR B 2
C43 C 0.6384(11) 0.3419(5) 0.7009(16) 0.053(3) Uiso 0.30 1 d P B 2
H43A H 0.5700 0.3462 0.6480 0.064 Uiso 0.30 1 calc PR B 2
H43B H 0.6407 0.3117 0.7550 0.064 Uiso 0.30 1 calc PR B 2
C44 C 0.652(2) 0.3726(10) 0.801(3) 0.071(6) Uiso 0.20 1 d P B 2
H44A H 0.5901 0.3859 0.8110 0.085 Uiso 0.20 1 calc PR B 2
H44B H 0.6925 0.3985 0.7773 0.085 Uiso 0.20 1 calc PR B 2
C45 C 0.7106(12) 0.3448(6) 0.9629(19) 0.059(4) Uiso 0.25 1 d P B 2
H45A H 0.6921 0.3597 1.0472 0.089 Uiso 0.25 1 calc PR B 2
H45B H 0.7805 0.3475 0.9754 0.089 Uiso 0.25 1 calc PR B 2
H45C H 0.6923 0.3114 0.9580 0.089 Uiso 0.25 1 calc PR B 2
C46 C 0.5609(14) 0.3671(7) 0.720(2) 0.048(4) Uiso 0.20 1 d P C 3
H46A H 0.5289 0.3944 0.6639 0.072 Uiso 0.20 1 calc PR C 3
H46B H 0.5132 0.3422 0.7196 0.072 Uiso 0.20 1 calc PR C 3
H46C H 0.6108 0.3552 0.6726 0.072 Uiso 0.20 1 calc PR C 3
C47 C 0.6024(9) 0.3803(4) 0.8633(14) 0.038(2) Uiso 0.30 1 d P C 3
H47A H 0.6510 0.4054 0.8661 0.046 Uiso 0.30 1 calc PR C 3
H47B H 0.5531 0.3918 0.9137 0.046 Uiso 0.30 1 calc PR C 3
C48 C 0.6270(12) 0.3569(6) 0.901(2) 0.048(4) Uiso 0.25 1 d P C 3
H48A H 0.6586 0.3631 1.0051 0.072 Uiso 0.25 1 calc PR C 3
H48B H 0.6751 0.3460 0.8488 0.072 Uiso 0.25 1 calc PR C 3
H48C H 0.5778 0.3324 0.8956 0.072 Uiso 0.25 1 calc PR C 3
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 0.02091(10) 0.01358(10) 0.01757(10) -0.00058(7) 0.00304(7) 0.00092(7)
Pd2 0.02084(10) 0.01319(10) 0.01795(10) -0.00062(6) 0.00447(7) 0.00055(7)
C1 0.0220(12) 0.0145(11) 0.0218(12) -0.0024(9) 0.0063(10) -0.0024(9)
C2 0.0213(12) 0.0219(12) 0.0230(12) 0.0008(10) 0.0039(10) -0.0001(10)
C3 0.0280(14) 0.0277(14) 0.0214(12) -0.0042(10) 0.0063(11) -0.0047(11)
C4 0.0386(16) 0.0266(14) 0.0307(14) -0.0081(11) 0.0154(12) -0.0010(12)
C5 0.0348(15) 0.0172(12) 0.0326(14) 0.0009(11) 0.0120(12) 0.0046(11)
C6 0.0240(13) 0.0174(12) 0.0264(13) 0.0005(10) 0.0072(10) -0.0001(10)
C7 0.0249(13) 0.0209(12) 0.0268(13) 0.0044(10) 0.0071(11) 0.0054(10)
N1 0.0239(11) 0.0175(10) 0.0207(10) 0.0008(8) 0.0044(8) 0.0006(8)
C8 0.0374(15) 0.0269(14) 0.0198(13) 0.0031(10) 0.0021(11) 0.0016(12)
C9 0.0313(14) 0.0229(13) 0.0315(14) 0.0042(11) 0.0097(12) -0.0026(11)
N2 0.0209(10) 0.0168(10) 0.0189(10) -0.0010(8) 0.0048(8) 0.0009(8)
C10 0.0230(12) 0.0176(12) 0.0200(12) 0.0002(9) 0.0076(10) 0.0012(9)
C11 0.0196(12) 0.0213(12) 0.0259(13) -0.0015(10) 0.0073(10) 0.0022(10)
C12 0.0260(14) 0.0284(14) 0.0318(15) 0.0059(11) 0.0082(11) 0.0005(11)
C13 0.0307(15) 0.0244(14) 0.0462(17) 0.0035(12) 0.0128(13) -0.0038(11)
C14 0.0260(14) 0.0307(15) 0.0434(17) -0.0096(13) 0.0079(12) -0.0082(12)
C15 0.0281(15) 0.0400(17) 0.0318(15) -0.0044(13) 0.0018(12) -0.0054(12)
C16 0.0259(13) 0.0249(13) 0.0307(14) 0.0014(11) 0.0048(11) -0.0015(11)
C17 0.0230(13) 0.0190(12) 0.0291(13) 0.0011(10) 0.0013(10) 0.0024(10)
C18 0.0451(19) 0.0305(16) 0.064(2) 0.0047(15) 0.0252(17) 0.0108(14)
C19 0.058(2) 0.0318(18) 0.092(3) -0.0027(19) 0.032(2) 0.0166(17)
C20 0.0429(19) 0.0189(15) 0.097(3) 0.0037(17) 0.005(2) 0.0087(14)
C21 0.0324(17) 0.0339(18) 0.092(3) 0.0291(19) 0.0116(18) 0.0045(14)
C22 0.0287(15) 0.0327(16) 0.057(2) 0.0178(15) 0.0124(14) 0.0112(12)
O1 0.0390(11) 0.0184(9) 0.0244(9) -0.0008(7) 0.0121(8) 0.0024(8)
O2 0.0328(10) 0.0196(9) 0.0271(10) -0.0036(7) 0.0127(8) -0.0016(8)
C23 0.0243(13) 0.0233(13) 0.0217(12) -0.0023(10) 0.0046(10) 0.0006(10)
C24 0.0379(16) 0.0294(15) 0.0344(15) -0.0023(12) 0.0184(13) 0.0011(12)
C25 0.0236(12) 0.0148(11) 0.0187(12) 0.0047(9) 0.0039(10) 0.0052(9)
C26 0.0236(12) 0.0186(12) 0.0226(12) 0.0014(10) 0.0020(10) 0.0037(10)
C27 0.0353(15) 0.0224(13) 0.0187(12) 0.0003(10) 0.0064(11) 0.0084(11)
C28 0.0332(14) 0.0225(13) 0.0257(13) 0.0066(10) 0.0122(11) 0.0075(11)
C29 0.0246(13) 0.0210(13) 0.0291(13) 0.0059(10) 0.0066(11) 0.0022(10)
C30 0.0247(12) 0.0152(11) 0.0218(12) 0.0037(9) 0.0046(10) 0.0045(10)
C31 0.0254(13) 0.0191(12) 0.0242(13) 0.0003(10) 0.0051(10) -0.0021(10)
N3 0.0280(11) 0.0158(10) 0.0207(10) -0.0005(8) 0.0062(9) -0.0009(8)
C32 0.0382(16) 0.0284(14) 0.0207(13) -0.0062(11) 0.0055(11) -0.0065(12)
C33 0.0341(15) 0.0146(12) 0.0383(16) -0.0017(11) 0.0087(12) 0.0012(11)
_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 C1 1.973(2) . ?
Pd1 N2 1.994(2) . ?
Pd1 N1 2.088(2) . ?
Pd1 O1 2.1621(18) . ?
Pd1 Pd2 3.0526(3) . ?
Pd2 C25 1.974(2) . ?
Pd2 N2 1.998(2) . ?
Pd2 N3 2.090(2) . ?
Pd2 O2 2.1243(18) . ?
C1 C2 1.399(3) . ?
C1 C6 1.403(3) . ?
C2 C3 1.391(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.396(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.497(4) . ?
C7 N1 1.494(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N1 C8 1.479(3) . ?
N1 C9 1.481(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N2 C10 1.274(3) . ?
C10 C11 1.496(4) . ?
C10 C17 1.509(3) . ?
C11 C16 1.398(4) . ?
C11 C12 1.398(4) . ?
C12 C13 1.387(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.382(4) . ?
C17 C18 1.386(4) . ?
C18 C19 1.389(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.376(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.356(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.394(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
O1 C23 1.255(3) . ?
O2 C23 1.262(3) . ?
C23 C24 1.516(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.406(3) . ?
C25 C30 1.408(4) . ?
C26 C27 1.389(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.389(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.394(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.502(3) . ?
C31 N3 1.493(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
N3 C32 1.474(3) . ?
N3 C33 1.488(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.580(10) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.439(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.473(11) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.557(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.705(17) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.54(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.26(2) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.60(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.25(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.72(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.38(2) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 0.793(18) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
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
C1 Pd1 N2 99.29(9) . . ?
C1 Pd1 N1 82.75(9) . . ?
N2 Pd1 N1 175.23(8) . . ?
C1 Pd1 O1 168.38(9) . . ?
N2 Pd1 O1 88.51(7) . . ?
N1 Pd1 O1 90.14(8) . . ?
C1 Pd1 Pd2 115.82(7) . . ?
N2 Pd1 Pd2 40.16(6) . . ?
N1 Pd1 Pd2 135.09(6) . . ?
O1 Pd1 Pd2 75.65(5) . . ?
C25 Pd2 N2 96.52(9) . . ?
C25 Pd2 N3 83.17(9) . . ?
N2 Pd2 N3 177.20(8) . . ?
C25 Pd2 O2 174.21(9) . . ?
N2 Pd2 O2 89.02(8) . . ?
N3 Pd2 O2 91.21(8) . . ?
C25 Pd2 Pd1 103.00(7) . . ?
N2 Pd2 Pd1 40.06(6) . . ?
N3 Pd2 Pd1 142.72(6) . . ?
O2 Pd2 Pd1 82.33(5) . . ?
C2 C1 C6 118.1(2) . . ?
C2 C1 Pd1 128.36(19) . . ?
C6 C1 Pd1 113.43(18) . . ?
C3 C2 C1 120.7(2) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 120.5(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 119.9(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 121.1(2) . . ?
C5 C6 C7 121.9(2) . . ?
C1 C6 C7 117.0(2) . . ?
N1 C7 C6 108.8(2) . . ?
N1 C7 H7A 109.9 . . ?
C6 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C6 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C8 N1 C9 108.9(2) . . ?
C8 N1 C7 109.8(2) . . ?
C9 N1 C7 109.7(2) . . ?
C8 N1 Pd1 113.63(16) . . ?
C9 N1 Pd1 107.35(16) . . ?
C7 N1 Pd1 107.38(15) . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 N2 Pd1 132.72(18) . . ?
C10 N2 Pd2 123.23(17) . . ?
Pd1 N2 Pd2 99.78(9) . . ?
N2 C10 C11 123.7(2) . . ?
N2 C10 C17 121.4(2) . . ?
C11 C10 C17 114.8(2) . . ?
C16 C11 C12 118.0(2) . . ?
C16 C11 C10 119.7(2) . . ?
C12 C11 C10 122.3(2) . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C12 120.5(3) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C15 C14 C13 119.6(3) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 120.2(3) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C11 121.1(3) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C22 C17 C18 118.6(3) . . ?
C22 C17 C10 124.1(2) . . ?
C18 C17 C10 117.4(3) . . ?
C17 C18 C19 120.6(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C20 C19 C18 119.9(3) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C21 C20 C19 120.0(3) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.6(3) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C17 C22 C21 120.3(3) . . ?
C17 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C23 O1 Pd1 130.10(17) . . ?
C23 O2 Pd2 123.45(16) . . ?
O1 C23 O2 126.7(2) . . ?
O1 C23 C24 116.8(2) . . ?
O2 C23 C24 116.6(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 117.4(2) . . ?
C26 C25 Pd2 128.02(19) . . ?
C30 C25 Pd2 114.61(18) . . ?
C27 C26 C25 121.4(2) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C28 C27 C26 120.3(2) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 119.5(2) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C28 C29 C30 120.2(3) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C29 C30 C25 121.1(2) . . ?
C29 C30 C31 121.6(2) . . ?
C25 C30 C31 117.1(2) . . ?
N3 C31 C30 110.3(2) . . ?
N3 C31 H31A 109.6 . . ?
C30 C31 H31A 109.6 . . ?
N3 C31 H31B 109.6 . . ?
C30 C31 H31B 109.6 . . ?
H31A C31 H31B 108.1 . . ?
C32 N3 C33 109.4(2) . . ?
C32 N3 C31 110.1(2) . . ?
C33 N3 C31 110.1(2) . . ?
C32 N3 Pd2 113.87(16) . . ?
C33 N3 Pd2 103.35(16) . . ?
C31 N3 Pd2 109.80(15) . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C34 115.8(7) . . ?
C36 C35 H35A 108.3 . . ?
C34 C35 H35A 108.3 . . ?
C36 C35 H35B 108.3 . . ?
C34 C35 H35B 108.3 . . ?
H35A C35 H35B 107.4 . . ?
C35 C36 C37 120.2(7) . . ?
C35 C36 H36A 107.3 . . ?
C37 C36 H36A 107.3 . . ?
C35 C36 H36B 107.3 . . ?
C37 C36 H36B 107.3 . . ?
H36A C36 H36B 106.9 . . ?
C36 C37 C38 122.8(7) . . ?
C36 C37 H37A 106.6 . . ?
C38 C37 H37A 106.6 . . ?
C36 C37 H37B 106.6 . . ?
C38 C37 H37B 106.6 . . ?
H37A C37 H37B 106.6 . . ?
C37 C38 C39 131.6(8) . . ?
C37 C38 H38A 104.4 . . ?
C39 C38 H38A 104.4 . . ?
C37 C38 H38B 104.4 . . ?
C39 C38 H38B 104.4 . . ?
H38A C38 H38B 105.6 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C41 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C40 120.7(15) . . ?
C42 C41 H41A 107.2 . . ?
C40 C41 H41A 107.2 . . ?
C42 C41 H41B 107.2 . . ?
C40 C41 H41B 107.2 . . ?
H41A C41 H41B 106.8 . . ?
C41 C42 C43 127.3(14) . . ?
C41 C42 H42A 105.5 . . ?
C43 C42 H42A 105.5 . . ?
C41 C42 H42B 105.5 . . ?
C43 C42 H42B 105.5 . . ?
H42A C42 H42B 106.1 . . ?
C44 C43 C42 132.2(17) . . ?
C44 C43 H43A 104.2 . . ?
C42 C43 H43A 104.2 . . ?
C44 C43 H43B 104.2 . . ?
C42 C43 H43B 104.2 . . ?
H43A C43 H43B 105.5 . . ?
C43 C44 C45 107(2) . . ?
C43 C44 H44A 110.4 . . ?
C45 C44 H44A 110.4 . . ?
C43 C44 H44B 110.4 . . ?
C45 C44 H44B 110.4 . . ?
H44A C44 H44B 108.6 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C46 104(2) . . ?
C48 C47 H47A 111.0 . . ?
C46 C47 H47A 111.0 . . ?
C48 C47 H47B 111.0 . . ?
C46 C47 H47B 111.0 . . ?
H47A C47 H47B 109.0 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 26.40
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 0.809
_refine_diff_density_min -0.443
_refine_diff_density_rms 0.080