#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:59:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178763 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/17/4101770.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4101770
loop_
_publ_author_name
'Stephen M. Goldup'
'David A. Leigh'
'Paul R. McGonigal'
'Vicki E. Ronaldson'
'Alexandra M. Z. Slawin'
_publ_section_title
;
 Two Axles Threaded Using a Single Template Site: Active Metal Template
 Macrobicyclic [3]Rotaxanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              315
_journal_page_last               320
_journal_paper_doi               10.1021/ja9080716
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C51 H76 Cl2 N2 O6 Pd'
_chemical_formula_sum            'C51 H76 Cl2 N2 O6 Pd'
_chemical_formula_weight         990.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.806(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.431(5)
_cell_length_b                   21.805(6)
_cell_length_c                   12.751(4)
_cell_measurement_reflns_used    11672
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.7613
_cell_measurement_theta_min      1.1329
_cell_volume                     4997(2)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            47896
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.0800
_refine_diff_density_max         1.716
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0020(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9169
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1291P)²+12.5084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2379
_reflns_number_gt                8137
_reflns_number_total             9169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9080716_si_001.cif
_cod_data_source_block           35.PdCl2(MeCN).
_cod_original_cell_volume        4997(3)
_cod_database_code               4101770
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'
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 0.18857(2) 0.005385(19) 0.50186(3) 0.0456(2) Uani 1 1 d . . .
Cl1 Cl 0.20144(8) -0.08707(7) 0.42440(14) 0.0632(4) Uani 1 1 d . . .
Cl2 Cl 0.17443(8) 0.09957(7) 0.57372(11) 0.0587(4) Uani 1 1 d . . .
C1 C 0.1307(4) 0.1141(3) 0.1212(4) 0.0580(15) Uani 1 1 d . . .
H1A H 0.1195 0.1570 0.0974 0.070 Uiso 1 1 calc R . .
H1B H 0.0889 0.0986 0.1507 0.070 Uiso 1 1 calc R . .
O2 O 0.1981(3) 0.1125(2) 0.2034(3) 0.0656(12) Uani 1 1 d . . .
C3 C 0.1957(3) 0.0737(3) 0.2910(4) 0.0497(12) Uani 1 1 d . . .
H3A H 0.1752 0.0332 0.2643 0.060 Uiso 1 1 calc R . .
H3B H 0.1629 0.0917 0.3348 0.060 Uiso 1 1 calc R . .
C4 C 0.2725(3) 0.0661(3) 0.3582(4) 0.0514(13) Uani 1 1 d . . .
N5 N 0.2792(2) 0.0369(2) 0.4545(4) 0.0492(11) Uani 1 1 d . . .
C6 C 0.3465(3) 0.0277(4) 0.5192(5) 0.0658(17) Uani 1 1 d . . .
C7 C 0.4105(3) 0.0466(4) 0.4871(6) 0.088(3) Uani 1 1 d . . .
H7A H 0.4582 0.0396 0.5322 0.105 Uiso 1 1 calc R . .
C8 C 0.4037(4) 0.0758(5) 0.3883(5) 0.094(3) Uani 1 1 d . . .
H8A H 0.4469 0.0886 0.3654 0.112 Uiso 1 1 calc R . .
C9 C 0.3353(3) 0.0859(4) 0.3249(5) 0.070(2) Uani 1 1 d . . .
H9A H 0.3304 0.1064 0.2579 0.084 Uiso 1 1 calc R . .
C10 C 0.3486(3) -0.0067(4) 0.6222(6) 0.077(2) Uani 1 1 d . . .
H10A H 0.3225 0.0174 0.6683 0.092 Uiso 1 1 calc R . .
H10B H 0.3223 -0.0463 0.6056 0.092 Uiso 1 1 calc R . .
O11 O 0.4233(2) -0.0179(3) 0.6790(4) 0.0887(17) Uani 1 1 d . . .
C12 C 0.4483(3) 0.0189(3) 0.7730(5) 0.0598(15) Uani 1 1 d . . .
H12A H 0.4074 0.0250 0.8107 0.072 Uiso 1 1 calc R . .
H12B H 0.4647 0.0596 0.7526 0.072 Uiso 1 1 calc R . .
C13 C 0.5120(3) -0.0136(3) 0.8452(4) 0.0500(13) Uani 1 1 d . . .
C14 C 0.5856(3) 0.0042(3) 0.8554(5) 0.0533(14) Uani 1 1 d . . .
C15 C 0.6428(4) -0.0292(4) 0.9218(6) 0.074(2) Uani 1 1 d . . .
H15A H 0.6934 -0.0176 0.9292 0.089 Uiso 1 1 calc R . .
C16 C 0.6241(5) -0.0793(4) 0.9763(5) 0.084(2) Uani 1 1 d . . .
H16A H 0.6628 -0.1023 1.0209 0.101 Uiso 1 1 calc R . .
C17 C 0.5529(5) -0.0968(4) 0.9687(6) 0.081(2) Uani 1 1 d . . .
H17A H 0.5415 -0.1312 1.0078 0.097 Uiso 1 1 calc R . .
C18 C 0.4970(4) -0.0636(3) 0.9025(5) 0.0625(16) Uani 1 1 d . . .
O19 O 0.4228(3) -0.0779(2) 0.8880(4) 0.0818(15) Uani 1 1 d . . .
C20 C 0.4018(6) -0.1273(4) 0.9482(8) 0.110(4) Uani 1 1 d . . .
H20A H 0.4217 -0.1207 1.0261 0.132 Uiso 1 1 calc R . .
H20B H 0.4220 -0.1664 0.9274 0.132 Uiso 1 1 calc R . .
C21 C 0.3187(7) -0.1295(5) 0.9242(10) 0.143(5) Uani 1 1 d . . .
H21A H 0.2995 -0.0889 0.9397 0.172 Uiso 1 1 calc R . .
H21B H 0.3028 -0.1599 0.9722 0.172 Uiso 1 1 calc R . .
C22 C 0.2853(7) -0.1465(6) 0.8085(11) 0.175(7) Uani 1 1 d D . .
H22A H 0.2887 -0.1099 0.7637 0.210 Uiso 1 1 calc R . .
H22B H 0.3173 -0.1785 0.7872 0.210 Uiso 1 1 calc R . .
C23 C 0.2065(6) -0.1691(6) 0.779(2) 0.39(2) Uani 1 1 d D . .
H23A H 0.2079 -0.2075 0.8210 0.468 Uiso 1 1 calc R . .
H23B H 0.1790 -0.1393 0.8146 0.468 Uiso 1 1 calc R . .
C24 C 0.1534(16) -0.1830(17) 0.6749(19) 0.69(5) Uani 1 1 d DU . .
H24A H 0.1074 -0.2044 0.6821 0.830 Uiso 1 1 calc R . .
H24B H 0.1427 -0.1481 0.6243 0.830 Uiso 1 1 calc R . .
C25 C 0.2147(18) -0.2244(13) 0.6583(18) 0.37(2) Uani 1 1 d DU . .
H25A H 0.2568 -0.2017 0.6399 0.447 Uiso 1 1 calc R . .
H25B H 0.2330 -0.2520 0.7201 0.447 Uiso 1 1 calc R . .
C26 C 0.1680(9) -0.2570(7) 0.564(3) 0.36(2) Uani 1 1 d DU . .
H26A H 0.1670 -0.3008 0.5837 0.432 Uiso 1 1 calc R . .
H26B H 0.1950 -0.2546 0.5048 0.432 Uiso 1 1 calc R . .
C27 C 0.0890(9) -0.2386(6) 0.5165(9) 0.159(6) Uani 1 1 d D . .
H27A H 0.0869 -0.1934 0.5215 0.191 Uiso 1 1 calc R . .
H27B H 0.0585 -0.2552 0.5649 0.191 Uiso 1 1 calc R . .
C28 C 0.0498(6) -0.2556(5) 0.4033(10) 0.225(11) Uani 1 1 d D . .
H28A H 0.0871 -0.2503 0.3588 0.270 Uiso 1 1 calc R . .
H28B H 0.0400 -0.3002 0.4048 0.270 Uiso 1 1 calc R . .
C29 C -0.0208(6) -0.2273(4) 0.3403(9) 0.127(4) Uani 1 1 d D . .
H29A H -0.0601 -0.2309 0.3817 0.153 Uiso 1 1 calc R . .
H29B H -0.0375 -0.2499 0.2718 0.153 Uiso 1 1 calc R . .
C30 C -0.0097(5) -0.1591(4) 0.3158(6) 0.085(2) Uani 1 1 d . . .
H30A H -0.0577 -0.1375 0.3092 0.102 Uiso 1 1 calc R . .
H30B H 0.0260 -0.1409 0.3775 0.102 Uiso 1 1 calc R . .
C31 C 0.0181(4) -0.1478(3) 0.2158(5) 0.0647(16) Uani 1 1 d . . .
H31A H -0.0194 -0.1630 0.1531 0.078 Uiso 1 1 calc R . .
H31B H 0.0644 -0.1716 0.2197 0.078 Uiso 1 1 calc R . .
C32 C 0.0335(3) -0.0808(2) 0.1988(4) 0.0540(13) Uani 1 1 d . . .
H32A H -0.0138 -0.0576 0.1862 0.065 Uiso 1 1 calc R . .
H32B H 0.0666 -0.0643 0.2647 0.065 Uiso 1 1 calc R . .
C33 C 0.0696(4) -0.0713(2) 0.1045(5) 0.0563(14) Uani 1 1 d . . .
H33A H 0.1148 -0.0969 0.1128 0.068 Uiso 1 1 calc R . .
H33B H 0.0347 -0.0828 0.0366 0.068 Uiso 1 1 calc R . .
O34 O 0.0888(3) -0.00708(17) 0.1025(3) 0.0568(10) Uani 1 1 d . . .
C35 C 0.1197(3) 0.0133(3) 0.0213(4) 0.0516(13) Uani 1 1 d . . .
C36 C 0.1386(3) 0.0752(3) 0.0263(4) 0.0500(12) Uani 1 1 d . . .
C37 C 0.1670(4) 0.1000(3) -0.0572(4) 0.0577(14) Uani 1 1 d . . .
C38 C 0.1785(4) 0.0645(3) -0.1426(4) 0.0631(16) Uani 1 1 d . . .
H38A H 0.1974 0.0820 -0.1994 0.076 Uiso 1 1 calc R . .
C39 C 0.1618(4) 0.0031(3) -0.1420(5) 0.0644(18) Uani 1 1 d . . .
H39A H 0.1708 -0.0220 -0.1987 0.077 Uiso 1 1 calc R . .
C40 C 0.1324(3) -0.0237(3) -0.0626(4) 0.0580(14) Uani 1 1 d . . .
H40A H 0.1211 -0.0662 -0.0647 0.070 Uiso 1 1 calc R . .
O41 O 0.5958(2) 0.0550(2) 0.7993(4) 0.0752(13) Uani 1 1 d . . .
C42 C 0.6712(4) 0.0722(4) 0.7971(8) 0.096(3) Uani 1 1 d . . .
H42A H 0.6946 0.0397 0.7614 0.115 Uiso 1 1 calc R . .
H42B H 0.7010 0.0774 0.8713 0.115 Uiso 1 1 calc R . .
C43 C 0.6690(6) 0.1295(4) 0.7381(9) 0.104(3) Uani 1 1 d . . .
H43A H 0.7202 0.1408 0.7333 0.125 Uiso 1 1 calc R . .
H43B H 0.6498 0.1624 0.7783 0.125 Uiso 1 1 calc R . .
C44 C 0.6214(5) 0.1258(3) 0.6280(9) 0.099(3) Uani 1 1 d . . .
H44A H 0.5689 0.1216 0.6338 0.119 Uiso 1 1 calc R . .
H44B H 0.6347 0.0881 0.5932 0.119 Uiso 1 1 calc R . .
C45 C 0.6272(6) 0.1798(4) 0.5561(9) 0.103(3) Uani 1 1 d . . .
H45A H 0.6192 0.2180 0.5939 0.124 Uiso 1 1 calc R . .
H45B H 0.6782 0.1812 0.5432 0.124 Uiso 1 1 calc R . .
C46 C 0.5750(6) 0.1779(4) 0.4544(9) 0.106(3) Uani 1 1 d . . .
H46A H 0.5241 0.1813 0.4672 0.127 Uiso 1 1 calc R . .
H46B H 0.5790 0.1375 0.4207 0.127 Uiso 1 1 calc R . .
C47 C 0.5854(12) 0.2263(6) 0.3786(9) 0.188(8) Uani 1 1 d . . .
H47A H 0.5806 0.2665 0.4124 0.225 Uiso 1 1 calc R . .
H47B H 0.6368 0.2234 0.3678 0.225 Uiso 1 1 calc R . .
C48 C 0.5368(7) 0.2252(7) 0.2785(12) 0.155(5) Uani 1 1 d D . .
H48A H 0.5251 0.1822 0.2565 0.186 Uiso 1 1 calc R . .
H48B H 0.5610 0.2445 0.2247 0.186 Uiso 1 1 calc R . .
C49 C 0.4665(7) 0.2587(10) 0.2809(10) 0.288(14) Uani 1 1 d DU . .
H49A H 0.4791 0.2989 0.3163 0.346 Uiso 1 1 calc R . .
H49B H 0.4382 0.2350 0.3245 0.346 Uiso 1 1 calc R . .
C50 C 0.4183(6) 0.2689(14) 0.1712(10) 0.301(14) Uani 1 1 d DU . .
H50A H 0.4187 0.2321 0.1259 0.361 Uiso 1 1 calc R . .
H50B H 0.4372 0.3042 0.1360 0.361 Uiso 1 1 calc R . .
C51 C 0.3408(5) 0.2817(6) 0.1841(7) 0.129(4) Uani 1 1 d D . .
H51A H 0.3343 0.3266 0.1879 0.155 Uiso 1 1 calc R . .
H51B H 0.3351 0.2641 0.2534 0.155 Uiso 1 1 calc R . .
C52 C 0.2799(5) 0.2566(4) 0.0960(6) 0.087(2) Uani 1 1 d D . .
H52A H 0.2823 0.2112 0.0988 0.104 Uiso 1 1 calc R . .
H52B H 0.2314 0.2689 0.1106 0.104 Uiso 1 1 calc R . .
C53 C 0.2821(4) 0.2764(4) -0.0145(6) 0.082(2) Uani 1 1 d . . .
H53A H 0.3277 0.2592 -0.0319 0.098 Uiso 1 1 calc R . .
H53B H 0.2872 0.3216 -0.0140 0.098 Uiso 1 1 calc R . .
C54 C 0.2168(4) 0.2593(3) -0.1049(5) 0.0687(18) Uani 1 1 d . . .
H54A H 0.2217 0.2821 -0.1701 0.082 Uiso 1 1 calc R . .
H54B H 0.1706 0.2737 -0.0852 0.082 Uiso 1 1 calc R . .
C55 C 0.2074(4) 0.1916(3) -0.1336(5) 0.0676(17) Uani 1 1 d . . .
H55A H 0.1709 0.1864 -0.2028 0.081 Uiso 1 1 calc R . .
H55B H 0.2555 0.1739 -0.1410 0.081 Uiso 1 1 calc R . .
O56 O 0.1816(3) 0.1611(2) -0.0485(3) 0.0675(12) Uani 1 1 d . . .
N57 N 0.1013(2) -0.0273(2) 0.5551(4) 0.0541(11) Uani 1 1 d . . .
C58 C 0.0560(3) -0.0478(3) 0.5918(4) 0.0505(13) Uani 1 1 d . . .
C59 C -0.0023(4) -0.0742(3) 0.6387(6) 0.0676(17) Uani 1 1 d . . .
H59A H -0.0435 -0.0881 0.5811 0.101 Uiso 1 1 calc R . .
H59B H -0.0204 -0.0430 0.6821 0.101 Uiso 1 1 calc R . .
H59C H 0.0178 -0.1091 0.6844 0.101 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N57 Pd1 N5 177.48(18) . . ?
N57 Pd1 Cl1 90.03(16) . . ?
N5 Pd1 Cl1 89.94(13) . . ?
N57 Pd1 Cl2 90.71(16) . . ?
N5 Pd1 Cl2 89.40(13) . . ?
Cl1 Pd1 Cl2 178.01(6) . . ?
O2 C1 C36 110.5(5) . . ?
O2 C1 H1A 109.6 . . ?
C36 C1 H1A 109.6 . . ?
O2 C1 H1B 109.6 . . ?
C36 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C3 O2 C1 114.7(4) . . ?
O2 C3 C4 109.1(4) . . ?
O2 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
O2 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N5 C4 C9 120.4(6) . . ?
N5 C4 C3 116.9(4) . . ?
C9 C4 C3 122.7(5) . . ?
C6 N5 C4 120.6(5) . . ?
C6 N5 Pd1 118.6(4) . . ?
C4 N5 Pd1 120.8(3) . . ?
N5 C6 C7 120.1(7) . . ?
N5 C6 C10 116.9(5) . . ?
C7 C6 C10 122.9(6) . . ?
C6 C7 C8 119.2(6) . . ?
C6 C7 H7A 120.4 . . ?
C8 C7 H7A 120.4 . . ?
C9 C8 C7 120.0(6) . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C8 C9 C4 119.7(7) . . ?
C8 C9 H9A 120.2 . . ?
C4 C9 H9A 120.2 . . ?
O11 C10 C6 111.4(6) . . ?
O11 C10 H10A 109.4 . . ?
C6 C10 H10A 109.4 . . ?
O11 C10 H10B 109.4 . . ?
C6 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 O11 C10 115.1(5) . . ?
O11 C12 C13 108.1(5) . . ?
O11 C12 H12A 110.1 . . ?
C13 C12 H12A 110.1 . . ?
O11 C12 H12B 110.1 . . ?
C13 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
C18 C13 C14 118.7(6) . . ?
C18 C13 C12 118.6(6) . . ?
C14 C13 C12 122.7(6) . . ?
O41 C14 C13 115.2(5) . . ?
O41 C14 C15 124.8(6) . . ?
C13 C14 C15 120.0(6) . . ?
C16 C15 C14 118.5(6) . . ?
C16 C15 H15A 120.7 . . ?
C14 C15 H15A 120.7 . . ?
C17 C16 C15 122.4(7) . . ?
C17 C16 H16A 118.8 . . ?
C15 C16 H16A 118.8 . . ?
C16 C17 C18 118.5(7) . . ?
C16 C17 H17A 120.7 . . ?
C18 C17 H17A 120.7 . . ?
O19 C18 C13 114.8(6) . . ?
O19 C18 C17 123.3(7) . . ?
C13 C18 C17 121.9(7) . . ?
C18 O19 C20 118.6(7) . . ?
O19 C20 C21 107.6(9) . . ?
O19 C20 H20A 110.2 . . ?
C21 C20 H20A 110.2 . . ?
O19 C20 H20B 110.2 . . ?
C21 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
C20 C21 C22 112.6(8) . . ?
C20 C21 H21A 109.1 . . ?
C22 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
C22 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C23 C22 C21 119.0(13) . . ?
C23 C22 H22A 107.6 . . ?
C21 C22 H22A 107.6 . . ?
C23 C22 H22B 107.6 . . ?
C21 C22 H22B 107.6 . . ?
H22A C22 H22B 107.0 . . ?
C24 C23 C22 134(2) . . ?
C24 C23 C25 48.3(8) . . ?
C22 C23 C25 98.9(13) . . ?
C24 C23 H23A 103.7 . . ?
C22 C23 H23A 103.7 . . ?
C25 C23 H23A 84.6 . . ?
C24 C23 H23B 103.7 . . ?
C22 C23 H23B 103.7 . . ?
C25 C23 H23B 152.1 . . ?
H23A C23 H23B 105.4 . . ?
C25 C24 C23 83.3(15) . . ?
C25 C24 H24A 114.8 . . ?
C23 C24 H24A 114.8 . . ?
C25 C24 H24B 114.8 . . ?
C23 C24 H24B 114.8 . . ?
H24A C24 H24B 111.8 . . ?
C26 C25 C24 95(2) . . ?
C26 C25 C23 142(2) . . ?
C24 C25 C23 48.4(8) . . ?
C26 C25 H25A 112.8 . . ?
C24 C25 H25A 112.8 . . ?
C23 C25 H25A 94.5 . . ?
C26 C25 H25B 112.8 . . ?
C24 C25 H25B 112.8 . . ?
C23 C25 H25B 79.7 . . ?
H25A C25 H25B 110.2 . . ?
C25 C26 C27 122(2) . . ?
C25 C26 H26A 106.8 . . ?
C27 C26 H26A 106.8 . . ?
C25 C26 H26B 106.8 . . ?
C27 C26 H26B 106.8 . . ?
H26A C26 H26B 106.7 . . ?
C26 C27 C28 122(2) . . ?
C26 C27 H27A 106.8 . . ?
C28 C27 H27A 106.8 . . ?
C26 C27 H27B 106.8 . . ?
C28 C27 H27B 106.8 . . ?
H27A C27 H27B 106.6 . . ?
C29 C28 C27 125.8(13) . . ?
C29 C28 H28A 105.9 . . ?
C27 C28 H28A 105.9 . . ?
C29 C28 H28B 105.9 . . ?
C27 C28 H28B 105.9 . . ?
H28A C28 H28B 106.2 . . ?
C28 C29 C30 111.5(8) . . ?
C28 C29 H29A 109.3 . . ?
C30 C29 H29A 109.3 . . ?
C28 C29 H29B 109.3 . . ?
C30 C29 H29B 109.3 . . ?
H29A C29 H29B 108.0 . . ?
C31 C30 C29 114.6(8) . . ?
C31 C30 H30A 108.6 . . ?
C29 C30 H30A 108.6 . . ?
C31 C30 H30B 108.6 . . ?
C29 C30 H30B 108.6 . . ?
H30A C30 H30B 107.6 . . ?
C30 C31 C32 113.1(6) . . ?
C30 C31 H31A 109.0 . . ?
C32 C31 H31A 109.0 . . ?
C30 C31 H31B 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C33 C32 C31 112.1(5) . . ?
C33 C32 H32A 109.2 . . ?
C31 C32 H32A 109.2 . . ?
C33 C32 H32B 109.2 . . ?
C31 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
O34 C33 C32 107.4(4) . . ?
O34 C33 H33A 110.2 . . ?
C32 C33 H33A 110.2 . . ?
O34 C33 H33B 110.2 . . ?
C32 C33 H33B 110.2 . . ?
H33A C33 H33B 108.5 . . ?
C35 O34 C33 118.3(4) . . ?
O34 C35 C36 115.1(5) . . ?
O34 C35 C40 124.1(6) . . ?
C36 C35 C40 120.8(6) . . ?
C35 C36 C37 118.2(5) . . ?
C35 C36 C1 120.9(5) . . ?
C37 C36 C1 120.8(5) . . ?
O56 C37 C38 123.2(5) . . ?
O56 C37 C36 114.8(5) . . ?
C38 C37 C36 122.0(6) . . ?
C39 C38 C37 117.7(6) . . ?
C39 C38 H38A 121.2 . . ?
C37 C38 H38A 121.2 . . ?
C38 C39 C40 122.8(6) . . ?
C38 C39 H39A 118.6 . . ?
C40 C39 H39A 118.6 . . ?
C39 C40 C35 118.4(6) . . ?
C39 C40 H40A 120.8 . . ?
C35 C40 H40A 120.8 . . ?
C14 O41 C42 118.0(6) . . ?
O41 C42 C43 108.4(8) . . ?
O41 C42 H42A 110.0 . . ?
C43 C42 H42A 110.0 . . ?
O41 C42 H42B 110.0 . . ?
C43 C42 H42B 110.0 . . ?
H42A C42 H42B 108.4 . . ?
C42 C43 C44 112.6(7) . . ?
C42 C43 H43A 109.1 . . ?
C44 C43 H43A 109.1 . . ?
C42 C43 H43B 109.1 . . ?
C44 C43 H43B 109.1 . . ?
H43A C43 H43B 107.8 . . ?
C43 C44 C45 115.1(8) . . ?
C43 C44 H44A 108.5 . . ?
C45 C44 H44A 108.5 . . ?
C43 C44 H44B 108.5 . . ?
C45 C44 H44B 108.5 . . ?
H44A C44 H44B 107.5 . . ?
C46 C45 C44 113.8(8) . . ?
C46 C45 H45A 108.8 . . ?
C44 C45 H45A 108.8 . . ?
C46 C45 H45B 108.8 . . ?
C44 C45 H45B 108.8 . . ?
H45A C45 H45B 107.7 . . ?
C45 C46 C47 114.5(10) . . ?
C45 C46 H46A 108.6 . . ?
C47 C46 H46A 108.6 . . ?
C45 C46 H46B 108.6 . . ?
C47 C46 H46B 108.6 . . ?
H46A C46 H46B 107.6 . . ?
C48 C47 C46 116.2(15) . . ?
C48 C47 H47A 108.2 . . ?
C46 C47 H47A 108.2 . . ?
C48 C47 H47B 108.2 . . ?
C46 C47 H47B 108.2 . . ?
H47A C47 H47B 107.4 . . ?
C47 C48 C49 111.0(12) . . ?
C47 C48 H48A 109.4 . . ?
C49 C48 H48A 109.4 . . ?
C47 C48 H48B 109.4 . . ?
C49 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C48 C49 C50 113.0(12) . . ?
C48 C49 H49A 109.0 . . ?
C50 C49 H49A 109.0 . . ?
C48 C49 H49B 109.0 . . ?
C50 C49 H49B 109.0 . . ?
H49A C49 H49B 107.8 . . ?
C49 C50 C51 107.9(9) . . ?
C49 C50 H50A 110.1 . . ?
C51 C50 H50A 110.1 . . ?
C49 C50 H50B 110.1 . . ?
C51 C50 H50B 110.1 . . ?
H50A C50 H50B 108.4 . . ?
C50 C51 C52 114.9(10) . . ?
C50 C51 H51A 108.5 . . ?
C52 C51 H51A 108.5 . . ?
C50 C51 H51B 108.5 . . ?
C52 C51 H51B 108.5 . . ?
H51A C51 H51B 107.5 . . ?
C53 C52 C51 115.5(7) . . ?
C53 C52 H52A 108.4 . . ?
C51 C52 H52A 108.4 . . ?
C53 C52 H52B 108.4 . . ?
C51 C52 H52B 108.4 . . ?
H52A C52 H52B 107.5 . . ?
C52 C53 C54 117.8(7) . . ?
C52 C53 H53A 107.9 . . ?
C54 C53 H53A 107.9 . . ?
C52 C53 H53B 107.9 . . ?
C54 C53 H53B 107.9 . . ?
H53A C53 H53B 107.2 . . ?
C53 C54 C55 116.7(6) . . ?
C53 C54 H54A 108.1 . . ?
C55 C54 H54A 108.1 . . ?
C53 C54 H54B 108.1 . . ?
C55 C54 H54B 108.1 . . ?
H54A C54 H54B 107.3 . . ?
O56 C55 C54 107.8(5) . . ?
O56 C55 H55A 110.2 . . ?
C54 C55 H55A 110.2 . . ?
O56 C55 H55B 110.2 . . ?
C54 C55 H55B 110.2 . . ?
H55A C55 H55B 108.5 . . ?
C37 O56 C55 118.9(5) . . ?
C58 N57 Pd1 174.4(4) . . ?
N57 C58 C59 179.8(7) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
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 N57 2.010(5) . ?
Pd1 N5 2.018(4) . ?
Pd1 Cl1 2.2804(16) . ?
Pd1 Cl2 2.2873(16) . ?
C1 O2 1.437(8) . ?
C1 C36 1.511(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
O2 C3 1.410(6) . ?
C3 C4 1.493(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N5 1.365(7) . ?
C4 C9 1.387(7) . ?
N5 C6 1.344(8) . ?
C6 C7 1.394(9) . ?
C6 C10 1.505(10) . ?
C7 C8 1.392(12) . ?
C7 H7A 0.9500 . ?
C8 C9 1.357(10) . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?
C10 O11 1.428(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O11 C12 1.432(8) . ?
C12 C13 1.499(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.375(9) . ?
C13 C14 1.389(8) . ?
C14 O41 1.353(8) . ?
C14 C15 1.402(9) . ?
C15 C16 1.380(11) . ?
C15 H15A 0.9500 . ?
C16 C17 1.350(12) . ?
C16 H16A 0.9500 . ?
C17 C18 1.383(10) . ?
C17 H17A 0.9500 . ?
C18 O19 1.374(8) . ?
O19 C20 1.425(9) . ?
C20 C21 1.495(15) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.513(17) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.500(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.499(5) . ?
C23 C25 1.99(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.498(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.50(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.500(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.510(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.502(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.542(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.495(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.514(8) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.512(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 O34 1.445(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O34 C35 1.364(7) . ?
C35 C36 1.392(8) . ?
C35 C40 1.401(8) . ?
C36 C37 1.394(8) . ?
C37 O56 1.358(8) . ?
C37 C38 1.392(8) . ?
C38 C39 1.374(9) . ?
C38 H38A 0.9500 . ?
C39 C40 1.379(9) . ?
C39 H39A 0.9500 . ?
C40 H40A 0.9500 . ?
O41 C42 1.447(8) . ?
C42 C43 1.454(13) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.483(14) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.511(12) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.433(14) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.472(16) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.388(17) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.493(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.498(5) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.501(5) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.504(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.482(9) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.518(11) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.523(10) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 O56 1.442(7) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
N57 C58 1.136(7) . ?
C58 C59 1.458(8) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C36 C1 O2 C3 -102.0(5) . . . . ?
C1 O2 C3 C4 168.4(4) . . . . ?
O2 C3 C4 N5 171.1(5) . . . . ?
O2 C3 C4 C9 -10.7(8) . . . . ?
C9 C4 N5 C6 1.0(8) . . . . ?
C3 C4 N5 C6 179.3(5) . . . . ?
C9 C4 N5 Pd1 -178.0(4) . . . . ?
C3 C4 N5 Pd1 0.3(6) . . . . ?
Cl1 Pd1 N5 C6 -87.6(4) . . . . ?
Cl2 Pd1 N5 C6 94.3(4) . . . . ?
Cl1 Pd1 N5 C4 91.4(4) . . . . ?
Cl2 Pd1 N5 C4 -86.7(4) . . . . ?
C4 N5 C6 C7 -1.6(9) . . . . ?
Pd1 N5 C6 C7 177.4(6) . . . . ?
C4 N5 C6 C10 -178.1(6) . . . . ?
Pd1 N5 C6 C10 0.9(8) . . . . ?
N5 C6 C7 C8 0.9(11) . . . . ?
C10 C6 C7 C8 177.2(7) . . . . ?
C6 C7 C8 C9 0.5(13) . . . . ?
C7 C8 C9 C4 -1.1(12) . . . . ?
N5 C4 C9 C8 0.3(10) . . . . ?
C3 C4 C9 C8 -177.8(6) . . . . ?
N5 C6 C10 O11 175.1(6) . . . . ?
C7 C6 C10 O11 -1.3(10) . . . . ?
C6 C10 O11 C12 106.4(7) . . . . ?
C10 O11 C12 C13 157.6(6) . . . . ?
O11 C12 C13 C18 -75.2(7) . . . . ?
O11 C12 C13 C14 104.1(7) . . . . ?
C18 C13 C14 O41 -177.8(5) . . . . ?
C12 C13 C14 O41 2.9(8) . . . . ?
C18 C13 C14 C15 1.0(8) . . . . ?
C12 C13 C14 C15 -178.2(5) . . . . ?
O41 C14 C15 C16 178.4(6) . . . . ?
C13 C14 C15 C16 -0.3(9) . . . . ?
C14 C15 C16 C17 -0.6(10) . . . . ?
C15 C16 C17 C18 0.8(11) . . . . ?
C14 C13 C18 O19 179.7(5) . . . . ?
C12 C13 C18 O19 -1.0(8) . . . . ?
C14 C13 C18 C17 -0.8(9) . . . . ?
C12 C13 C18 C17 178.4(6) . . . . ?
C16 C17 C18 O19 179.3(6) . . . . ?
C16 C17 C18 C13 -0.1(10) . . . . ?
C13 C18 O19 C20 -177.1(6) . . . . ?
C17 C18 O19 C20 3.4(9) . . . . ?
C18 O19 C20 C21 175.4(6) . . . . ?
O19 C20 C21 C22 66.1(12) . . . . ?
C20 C21 C22 C23 161.7(11) . . . . ?
C21 C22 C23 C24 172(2) . . . . ?
C21 C22 C23 C25 -149.4(16) . . . . ?
C22 C23 C24 C25 55(4) . . . . ?
C23 C24 C25 C26 168(2) . . . . ?
C24 C23 C25 C26 -20(4) . . . . ?
C22 C23 C25 C26 -163(4) . . . . ?
C22 C23 C25 C24 -143(3) . . . . ?
C24 C25 C26 C27 4(4) . . . . ?
C23 C25 C26 C27 19(5) . . . . ?
C25 C26 C27 C28 159(2) . . . . ?
C26 C27 C28 C29 -164.1(11) . . . . ?
C27 C28 C29 C30 65.4(16) . . . . ?
C28 C29 C30 C31 86.7(11) . . . . ?
C29 C30 C31 C32 -175.9(6) . . . . ?
C30 C31 C32 C33 173.6(6) . . . . ?
C31 C32 C33 O34 -174.2(5) . . . . ?
C32 C33 O34 C35 -177.5(5) . . . . ?
C33 O34 C35 C36 -178.3(5) . . . . ?
C33 O34 C35 C40 1.8(8) . . . . ?
O34 C35 C36 C37 -176.7(5) . . . . ?
C40 C35 C36 C37 3.2(9) . . . . ?
O34 C35 C36 C1 5.1(8) . . . . ?
C40 C35 C36 C1 -175.0(5) . . . . ?
O2 C1 C36 C35 89.8(6) . . . . ?
O2 C1 C36 C37 -88.4(6) . . . . ?
C35 C36 C37 O56 177.7(5) . . . . ?
C1 C36 C37 O56 -4.0(8) . . . . ?
C35 C36 C37 C38 -1.8(9) . . . . ?
C1 C36 C37 C38 176.5(6) . . . . ?
O56 C37 C38 C39 179.8(6) . . . . ?
C36 C37 C38 C39 -0.7(10) . . . . ?
C37 C38 C39 C40 1.9(10) . . . . ?
C38 C39 C40 C35 -0.5(10) . . . . ?
O34 C35 C40 C39 177.7(6) . . . . ?
C36 C35 C40 C39 -2.1(9) . . . . ?
C13 C14 O41 C42 -173.4(6) . . . . ?
C15 C14 O41 C42 7.8(9) . . . . ?
C14 O41 C42 C43 -176.7(6) . . . . ?
O41 C42 C43 C44 -56.3(9) . . . . ?
C42 C43 C44 C45 -169.8(7) . . . . ?
C43 C44 C45 C46 -173.8(8) . . . . ?
C44 C45 C46 C47 -173.4(10) . . . . ?
C45 C46 C47 C48 178.8(12) . . . . ?
C46 C47 C48 C49 85.8(18) . . . . ?
C47 C48 C49 C50 169.4(19) . . . . ?
C48 C49 C50 C51 160.3(17) . . . . ?
C49 C50 C51 C52 -144.6(17) . . . . ?
C50 C51 C52 C53 -55.8(17) . . . . ?
C51 C52 C53 C54 -172.2(8) . . . . ?
C52 C53 C54 C55 -68.6(9) . . . . ?
C53 C54 C55 O56 72.4(7) . . . . ?
C38 C37 O56 C55 2.6(9) . . . . ?
C36 C37 O56 C55 -176.8(5) . . . . ?
C54 C55 O56 C37 178.2(5) . . . . ?
