# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_C22H27N3O2(1)in_the_manuscript

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H27 N3 O2'
_chemical_formula_weight         365.47

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7711(8)
_cell_length_b                   21.7414(18)
_cell_length_c                   11.1390(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.364(2)
_cell_angle_gamma                90.00
_cell_volume                     2066.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2458
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      19.79

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18199
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         27.00
_reflns_number_total             4507
_reflns_number_gt                1497
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0570P)²+0.0000P] where P=(Fo²+2Fc²)/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         4507
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_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
N1 N 1.1556(3) 0.03820(9) 0.5545(2) 0.0913(7) Uani 1 1 d . . .
H1 H 1.1432 -0.0023 0.5508 0.110 Uiso 1 1 d R . .
N2 N 1.0280(2) 0.07297(11) 0.5081(2) 0.0922(7) Uani 1 1 d . . .
C3 C 1.0825(3) 0.13039(12) 0.5132(2) 0.0774(7) Uani 1 1 d . . .
C4 C 1.2440(3) 0.13062(12) 0.5623(2) 0.0840(7) Uani 1 1 d . . .
H4 H 1.3093 0.1649 0.5753 0.101 Uiso 1 1 calc R . .
C5 C 1.2874(3) 0.07121(13) 0.5874(2) 0.0779(7) Uani 1 1 d . . .
C6 C 1.4383(3) 0.04032(14) 0.6339(2) 0.0810(7) Uani 1 1 d . . .
C10 C 1.5667(4) -0.04815(14) 0.6985(3) 0.1104(9) Uani 1 1 d . . .
H10 H 1.5638 -0.0898 0.7167 0.133 Uiso 1 1 calc R . .
C9 C 1.7102(4) -0.02074(18) 0.7137(3) 0.1129(10) Uani 1 1 d . . .
H9 H 1.8017 -0.0431 0.7426 0.136 Uiso 1 1 calc R . .
C8 C 1.7161(3) 0.03993(18) 0.6855(3) 0.1177(10) Uani 1 1 d . . .
H8 H 1.8117 0.0599 0.6934 0.141 Uiso 1 1 calc R . .
C7 C 1.5776(3) 0.07102(13) 0.6453(3) 0.1041(9) Uani 1 1 d . . .
H7 H 1.5781 0.1126 0.6259 0.125 Uiso 1 1 calc R . .
C11 C 0.9754(3) 0.18186(12) 0.4692(2) 0.0757(7) Uani 1 1 d . . .
C12 C 1.0324(3) 0.24159(12) 0.4839(2) 0.0834(7) Uani 1 1 d . . .
H12 H 1.1371 0.2489 0.5212 0.100 Uiso 1 1 calc R . .
C13 C 0.9322(3) 0.29011(13) 0.4425(2) 0.0859(7) Uani 1 1 d . . .
C14 C 0.7748(3) 0.27982(13) 0.3847(2) 0.0893(8) Uani 1 1 d . . .
H14 H 0.7083 0.3124 0.3546 0.107 Uiso 1 1 calc R . .
C15 C 0.7212(3) 0.22036(14) 0.3736(2) 0.0853(7) Uani 1 1 d . . .
C16 C 0.8198(3) 0.17112(13) 0.4141(2) 0.0840(7) Uani 1 1 d . . .
H16 H 0.7816 0.1311 0.4042 0.101 Uiso 1 1 calc R . .
C17 C 0.4543(3) 0.25013(12) 0.2863(2) 0.1025(9) Uani 1 1 d . . .
H17A H 0.4780 0.2752 0.2209 0.123 Uiso 1 1 calc R . .
H17B H 0.4483 0.2765 0.3553 0.123 Uiso 1 1 calc R . .
C18 C 0.2991(3) 0.21480(13) 0.2399(3) 0.1070(9) Uani 1 1 d . . .
H18A H 0.3125 0.1860 0.1766 0.128 Uiso 1 1 calc R . .
H18B H 0.2775 0.1911 0.3078 0.128 Uiso 1 1 calc R . .
C19 C 0.1650(3) 0.25334(14) 0.1900(3) 0.1180(10) Uani 1 1 d . . .
H19A H 0.1859 0.2778 0.1228 0.142 Uiso 1 1 calc R . .
H19B H 0.1477 0.2812 0.2535 0.142 Uiso 1 1 calc R . .
C20 C 0.0188(3) 0.21509(15) 0.1431(3) 0.1291(11) Uani 1 1 d . . .
H20A H 0.0368 0.1866 0.0821 0.194 Uiso 1 1 calc R . .
H20B H -0.0671 0.2416 0.1071 0.194 Uiso 1 1 calc R . .
H20C H -0.0060 0.1928 0.2106 0.194 Uiso 1 1 calc R . .
C21 C 1.1321(3) 0.36539(11) 0.5186(3) 0.0951(8) Uani 1 1 d . . .
H21A H 1.2074 0.3487 0.4759 0.114 Uiso 1 1 calc R . .
H21B H 1.1528 0.3478 0.6009 0.114 Uiso 1 1 calc R . .
C22 C 1.1463(3) 0.43396(12) 0.5263(2) 0.0944(8) Uani 1 1 d . . .
H22A H 1.0696 0.4499 0.5686 0.113 Uiso 1 1 calc R . .
H22B H 1.1224 0.4508 0.4434 0.113 Uiso 1 1 calc R . .
C23 C 1.3070(3) 0.45520(13) 0.5931(3) 0.1182(10) Uani 1 1 d . . .
H23A H 1.3837 0.4386 0.5515 0.142 Uiso 1 1 calc R . .
H23B H 1.3301 0.4388 0.6763 0.142 Uiso 1 1 calc R . .
C24 C 1.3238(3) 0.52436(14) 0.5997(3) 0.1271(11) Uani 1 1 d . . .
H24A H 1.3074 0.5408 0.5177 0.191 Uiso 1 1 calc R . .
H24B H 1.4271 0.5349 0.6457 0.191 Uiso 1 1 calc R . .
H24C H 1.2475 0.5413 0.6399 0.191 Uiso 1 1 calc R . .
N3 N 1.4311(3) -0.01904(12) 0.6593(2) 0.0974(7) Uani 1 1 d . . .
O1 O 0.5692(2) 0.20400(8) 0.32318(17) 0.1104(7) Uani 1 1 d . . .
O2 O 0.97625(19) 0.35056(8) 0.45287(17) 0.1027(6) Uani 1 1 d . . .


_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
N1 C5 1.337(3) . ?
N1 N2 1.351(2) . ?
N1 H1 0.8870 . ?
N2 C3 1.334(3) . ?
C3 C4 1.395(3) . ?
C3 C11 1.470(3) . ?
C4 C5 1.357(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.468(3) . ?
C6 N3 1.326(3) . ?
C6 C7 1.372(3) . ?
C10 N3 1.329(3) . ?
C10 C9 1.367(4) . ?
C10 H10 0.9300 . ?
C9 C8 1.360(4) . ?
C9 H9 0.9300 . ?
C8 C7 1.372(3) . ?
C8 H8 0.9300 . ?
C7 H7 0.9300 . ?
C11 C16 1.381(3) . ?
C11 C12 1.388(3) . ?
C12 C13 1.382(3) . ?
C12 H12 0.9300 . ?
C13 O2 1.367(3) . ?
C13 C14 1.401(3) . ?
C14 C15 1.371(3) . ?
C14 H14 0.9300 . ?
C15 O1 1.368(3) . ?
C15 C16 1.385(3) . ?
C16 H16 0.9300 . ?
C17 O1 1.414(3) . ?
C17 C18 1.544(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.447(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.516(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O2 1.430(3) . ?
C21 C22 1.497(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.506(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.511(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

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
C5 N1 N2 113.1(2) . . ?
C5 N1 H1 129.4 . . ?
N2 N1 H1 117.1 . . ?
C3 N2 N1 104.48(19) . . ?
N2 C3 C4 110.0(2) . . ?
N2 C3 C11 120.2(2) . . ?
C4 C3 C11 129.8(3) . . ?
C5 C4 C3 106.7(2) . . ?
C5 C4 H4 126.6 . . ?
C3 C4 H4 126.6 . . ?
N1 C5 C4 105.7(2) . . ?
N1 C5 C6 120.2(2) . . ?
C4 C5 C6 134.0(3) . . ?
N3 C6 C7 122.6(2) . . ?
N3 C6 C5 115.9(2) . . ?
C7 C6 C5 121.4(3) . . ?
N3 C10 C9 124.2(3) . . ?
N3 C10 H10 117.9 . . ?
C9 C10 H10 117.9 . . ?
C8 C9 C10 118.5(3) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C9 C8 C7 118.4(3) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.8 . . ?
C8 C7 C6 119.5(3) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C16 C11 C12 120.2(2) . . ?
C16 C11 C3 120.6(2) . . ?
C12 C11 C3 119.2(2) . . ?
C13 C12 C11 119.4(2) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
O2 C13 C12 124.1(2) . . ?
O2 C13 C14 114.9(2) . . ?
C12 C13 C14 121.0(2) . . ?
C15 C14 C13 118.2(2) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
O1 C15 C14 124.3(2) . . ?
O1 C15 C16 114.1(2) . . ?
C14 C15 C16 121.6(2) . . ?
C11 C16 C15 119.5(2) . . ?
C11 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
O1 C17 C18 105.0(2) . . ?
O1 C17 H17A 110.8 . . ?
C18 C17 H17A 110.8 . . ?
O1 C17 H17B 110.8 . . ?
C18 C17 H17B 110.8 . . ?
H17A C17 H17B 108.8 . . ?
C19 C18 C17 114.6(2) . . ?
C19 C18 H18A 108.6 . . ?
C17 C18 H18A 108.6 . . ?
C19 C18 H18B 108.6 . . ?
C17 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C18 C19 C20 111.3(3) . . ?
C18 C19 H19A 109.4 . . ?
C20 C19 H19A 109.4 . . ?
C18 C19 H19B 109.4 . . ?
C20 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 C21 C22 108.1(2) . . ?
O2 C21 H21A 110.1 . . ?
C22 C21 H21A 110.1 . . ?
O2 C21 H21B 110.1 . . ?
C22 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
C21 C22 C23 112.9(2) . . ?
C21 C22 H22A 109.0 . . ?
C23 C22 H22A 109.0 . . ?
C21 C22 H22B 109.0 . . ?
C23 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C22 C23 C24 113.5(2) . . ?
C22 C23 H23A 108.9 . . ?
C24 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
C24 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
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 . . ?
C6 N3 C10 116.8(2) . . ?
C15 O1 C17 119.8(2) . . ?
C13 O2 C21 118.54(19) . . ?

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
C5 N1 N2 C3 -0.5(3) . . . . ?
N1 N2 C3 C4 0.3(3) . . . . ?
N1 N2 C3 C11 179.8(2) . . . . ?
N2 C3 C4 C5 0.0(3) . . . . ?
C11 C3 C4 C5 -179.4(2) . . . . ?
N2 N1 C5 C4 0.5(3) . . . . ?
N2 N1 C5 C6 -177.0(2) . . . . ?
C3 C4 C5 N1 -0.3(3) . . . . ?
C3 C4 C5 C6 176.7(2) . . . . ?
N1 C5 C6 N3 -10.5(3) . . . . ?
C4 C5 C6 N3 172.8(3) . . . . ?
N1 C5 C6 C7 167.0(2) . . . . ?
C4 C5 C6 C7 -9.7(4) . . . . ?
N3 C10 C9 C8 -1.0(5) . . . . ?
C10 C9 C8 C7 1.2(5) . . . . ?
C9 C8 C7 C6 -0.4(4) . . . . ?
N3 C6 C7 C8 -0.6(4) . . . . ?
C5 C6 C7 C8 -178.0(2) . . . . ?
N2 C3 C11 C16 -4.7(3) . . . . ?
C4 C3 C11 C16 174.6(2) . . . . ?
N2 C3 C11 C12 175.2(2) . . . . ?
C4 C3 C11 C12 -5.4(4) . . . . ?
C16 C11 C12 C13 -0.2(3) . . . . ?
C3 C11 C12 C13 179.9(2) . . . . ?
C11 C12 C13 O2 179.7(2) . . . . ?
C11 C12 C13 C14 -0.8(4) . . . . ?
O2 C13 C14 C15 -178.5(2) . . . . ?
C12 C13 C14 C15 2.0(4) . . . . ?
C13 C14 C15 O1 177.6(2) . . . . ?
C13 C14 C15 C16 -2.2(4) . . . . ?
C12 C11 C16 C15 0.0(3) . . . . ?
C3 C11 C16 C15 179.9(2) . . . . ?
O1 C15 C16 C11 -178.6(2) . . . . ?
C14 C15 C16 C11 1.3(4) . . . . ?
O1 C17 C18 C19 -176.5(2) . . . . ?
C17 C18 C19 C20 178.3(2) . . . . ?
O2 C21 C22 C23 -179.5(2) . . . . ?
C21 C22 C23 C24 179.1(2) . . . . ?
C7 C6 N3 C10 0.8(4) . . . . ?
C5 C6 N3 C10 178.3(2) . . . . ?
C9 C10 N3 C6 0.0(4) . . . . ?
C14 C15 O1 C17 -4.3(4) . . . . ?
C16 C15 O1 C17 175.5(2) . . . . ?
C18 C17 O1 C15 -177.7(2) . . . . ?
C12 C13 O2 C21 -4.9(4) . . . . ?
C14 C13 O2 C21 175.6(2) . . . . ?
C22 C21 O2 C13 -175.1(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 N2 0.89 2.14 2.899(3) 142.8 3_756

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.149
_refine_diff_density_rms         0.026
_database_code_depnum_ccdc_archive 'CCDC 977934'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_C68H100N6O4Pd1(2)in_the_manuscript


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H100 N6 O4 Pd'
_chemical_formula_weight         1171.94

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

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

_cell_length_a                   6.785(2)
_cell_length_b                   14.665(5)
_cell_length_c                   18.048(5)
_cell_angle_alpha                67.868(6)
_cell_angle_beta                 83.627(7)
_cell_angle_gamma                82.800(7)
_cell_volume                     1646.3(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    678
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      17.30

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             628
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11266
_diffrn_reflns_av_R_equivalents  0.1462
_diffrn_reflns_av_sigmaI/netI    0.3901
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.22
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5635
_reflns_number_gt                1597
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/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         5635
_refine_ls_number_parameters     346
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.2632
_refine_ls_R_factor_gt           0.0717
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1116
_refine_ls_goodness_of_fit_ref   0.851
_refine_ls_restrained_S_all      0.855
_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
C3 C 0.1459(13) 0.4310(6) 0.3592(6) 0.061(3) Uani 1 1 d . . .
C4 C 0.0596(12) 0.3885(5) 0.4350(5) 0.067(2) Uani 1 1 d . . .
H4 H -0.0534 0.3540 0.4488 0.080 Uiso 1 1 calc R . .
C5 C 0.1680(13) 0.4056(6) 0.4867(7) 0.067(2) Uani 1 1 d . . .
C11 C 0.0936(14) 0.4382(6) 0.2808(7) 0.068(3) Uani 1 1 d . . .
C12 C -0.0678(13) 0.3919(5) 0.2751(5) 0.070(3) Uani 1 1 d . . .
H12 H -0.1403 0.3558 0.3216 0.084 Uiso 1 1 calc R . .
C13 C -0.1218(13) 0.3983(6) 0.2022(6) 0.070(2) Uani 1 1 d . . .
C14 C -0.0160(12) 0.4512(6) 0.1330(5) 0.070(2) Uani 1 1 d . . .
H14 H -0.0488 0.4551 0.0831 0.084 Uiso 1 1 calc R . .
C15 C 0.1422(16) 0.4987(7) 0.1401(7) 0.078(3) Uani 1 1 d . . .
C16 C 0.2011(12) 0.4894(6) 0.2124(8) 0.072(3) Uani 1 1 d . . .
H16 H 0.3139 0.5178 0.2151 0.087 Uiso 1 1 calc R . .
C17 C -0.3878(12) 0.2950(6) 0.2622(5) 0.075(3) Uani 1 1 d . . .
H17A H -0.4561 0.3379 0.2885 0.090 Uiso 1 1 calc R . .
H17B H -0.3008 0.2452 0.2993 0.090 Uiso 1 1 calc R . .
C18 C -0.5369(12) 0.2465(5) 0.2357(5) 0.077(3) Uani 1 1 d . . .
H18A H -0.4672 0.2057 0.2077 0.092 Uiso 1 1 calc R . .
H18B H -0.6241 0.2969 0.1992 0.092 Uiso 1 1 calc R . .
C19 C -0.6607(11) 0.1825(6) 0.3094(5) 0.078(3) Uani 1 1 d . . .
H19A H -0.5714 0.1336 0.3460 0.093 Uiso 1 1 calc R . .
H19B H -0.7292 0.2241 0.3369 0.093 Uiso 1 1 calc R . .
C20 C -0.8130(12) 0.1299(6) 0.2889(5) 0.082(3) Uani 1 1 d . . .
H20A H -0.9012 0.1786 0.2516 0.098 Uiso 1 1 calc R . .
H20B H -0.7447 0.0871 0.2625 0.098 Uiso 1 1 calc R . .
C21 C -0.9376(12) 0.0680(6) 0.3631(5) 0.085(3) Uani 1 1 d . . .
H21A H -1.0096 0.1114 0.3883 0.102 Uiso 1 1 calc R . .
H21B H -0.8487 0.0213 0.4013 0.102 Uiso 1 1 calc R . .
C22 C -1.0865(12) 0.0112(5) 0.3442(4) 0.084(3) Uani 1 1 d D . .
H22A H -1.1753 0.0580 0.3060 0.101 Uiso 1 1 calc R . .
H22B H -1.0144 -0.0321 0.3189 0.101 Uiso 1 1 calc R . .
C23 C -1.2093(11) -0.0498(6) 0.4168(4) 0.093(3) Uani 1 1 d D . .
H23A H -1.2755 -0.0068 0.4435 0.111 Uiso 1 1 calc R . .
H23B H -1.1203 -0.0984 0.4537 0.111 Uiso 1 1 calc R . .
C24 C -1.3659(12) -0.1034(6) 0.3992(5) 0.092(3) Uani 1 1 d D . .
H24A H -1.4555 -0.0556 0.3620 0.111 Uiso 1 1 calc R . .
H24B H -1.3011 -0.1482 0.3740 0.111 Uiso 1 1 calc R . .
C25 C -1.4851(13) -0.1613(6) 0.4752(5) 0.119(4) Uani 1 1 d D . .
H25A H -1.5474 -0.1166 0.5009 0.143 Uiso 1 1 calc R . .
H25B H -1.3955 -0.2099 0.5119 0.143 Uiso 1 1 calc R . .
C26 C -1.6437(13) -0.2134(6) 0.4586(6) 0.162(5) Uani 1 1 d D . .
H26A H -1.7410 -0.1652 0.4271 0.243 Uiso 1 1 calc R . .
H26B H -1.7072 -0.2538 0.5084 0.243 Uiso 1 1 calc R . .
H26C H -1.5838 -0.2541 0.4297 0.243 Uiso 1 1 calc R . .
C27 C 0.4152(16) 0.5939(7) 0.0782(5) 0.122(4) Uani 1 1 d D . .
H27A H 0.3710 0.6372 0.1074 0.146 Uiso 1 1 calc R . .
H27B H 0.5088 0.5420 0.1099 0.146 Uiso 1 1 calc R . .
C28 C 0.5189(14) 0.6518(7) -0.0003(5) 0.114(4) Uani 1 1 d D . .
H28A H 0.4259 0.7018 -0.0341 0.137 Uiso 1 1 calc R . .
H28B H 0.5757 0.6085 -0.0281 0.137 Uiso 1 1 calc R . .
C29 C 0.6828(14) 0.7002(7) 0.0189(5) 0.111(4) Uani 1 1 d D . .
H29A H 0.6242 0.7380 0.0512 0.133 Uiso 1 1 calc R . .
H29B H 0.7772 0.6488 0.0506 0.133 Uiso 1 1 calc R . .
C30 C 0.7925(15) 0.7674(7) -0.0544(5) 0.129(4) Uani 1 1 d D . .
H30A H 0.6980 0.8168 -0.0878 0.155 Uiso 1 1 calc R . .
H30B H 0.8592 0.7291 -0.0851 0.155 Uiso 1 1 calc R . .
C31 C 0.9454(15) 0.8185(7) -0.0321(5) 0.120(4) Uani 1 1 d D . .
H31A H 0.8772 0.8547 -0.0001 0.144 Uiso 1 1 calc R . .
H31B H 1.0388 0.7682 0.0013 0.144 Uiso 1 1 calc R . .
C32 C 1.0621(15) 0.8891(8) -0.1019(5) 0.134(4) Uani 1 1 d D . .
H32A H 0.9684 0.9373 -0.1368 0.160 Uiso 1 1 calc R . .
H32B H 1.1356 0.8521 -0.1324 0.160 Uiso 1 1 calc R . .
C33 C 1.2067(16) 0.9439(8) -0.0803(6) 0.141(4) Uani 1 1 d D . .
H33A H 1.1317 0.9826 -0.0516 0.169 Uiso 1 1 calc R . .
H33B H 1.2963 0.8954 -0.0436 0.169 Uiso 1 1 calc R . .
C34 C 1.3310(17) 1.0120(7) -0.1483(5) 0.147(4) Uani 1 1 d D . .
H34A H 1.2420 1.0616 -0.1845 0.176 Uiso 1 1 calc R . .
H34B H 1.4046 0.9738 -0.1778 0.176 Uiso 1 1 calc R . .
C35 C 1.4773(17) 1.0642(9) -0.1246(6) 0.189(6) Uani 1 1 d D . .
H35A H 1.4043 1.1035 -0.0960 0.227 Uiso 1 1 calc R . .
H35B H 1.5662 1.0149 -0.0881 0.227 Uiso 1 1 calc R . .
C36 C 1.6008(16) 1.1307(8) -0.1945(6) 0.195(6) Uani 1 1 d D . .
H36A H 1.6933 1.0910 -0.2168 0.292 Uiso 1 1 calc R . .
H36B H 1.6727 1.1698 -0.1764 0.292 Uiso 1 1 calc R . .
H36C H 1.5149 1.1735 -0.2348 0.292 Uiso 1 1 calc R . .
N1 N 0.3233(10) 0.4582(5) 0.4447(6) 0.080(3) Uani 1 1 d . . .
N2 N 0.3097(11) 0.4728(5) 0.3663(5) 0.075(2) Uani 1 1 d . . .
O1 O -0.2751(9) 0.3510(4) 0.1911(3) 0.0826(19) Uani 1 1 d . . .
O2 O 0.2449(10) 0.5499(5) 0.0681(4) 0.097(2) Uani 1 1 d . . .
Pd1 Pd 0.5000 0.5000 0.5000 0.0654(5) Uani 1 2 d S . .
C6 C 0.1672(16) 0.3851(7) 0.5724(7) 0.071(3) Uani 1 1 d . . .
C7 C 0.0323(15) 0.3353(7) 0.6277(7) 0.083(3) Uani 1 1 d . . .
H7 H -0.0708 0.3125 0.6114 0.100 Uiso 1 1 calc R . .
C8 C 0.0411(15) 0.3163(6) 0.7088(7) 0.089(3) Uani 1 1 d . . .
H8 H -0.0505 0.2795 0.7472 0.106 Uiso 1 1 calc R . .
C9 C 0.1930(18) 0.3549(7) 0.7293(6) 0.097(4) Uani 1 1 d . . .
H9 H 0.2028 0.3459 0.7827 0.116 Uiso 1 1 calc R . .
C10 C 0.3318(14) 0.4073(7) 0.6705(7) 0.075(3) Uani 1 1 d . . .
H10 H 0.4353 0.4324 0.6844 0.091 Uiso 1 1 calc R . .
N3 N 0.3140(10) 0.4211(4) 0.5927(5) 0.064(2) Uani 1 1 d . . .


_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
C3 N2 1.374(8) . ?
C3 C4 1.370(9) . ?
C3 C11 1.458(10) . ?
C4 C5 1.359(10) . ?
C4 H4 0.9300 . ?
C5 N1 1.366(9) . ?
C5 C6 1.459(11) . ?
C11 C16 1.364(10) . ?
C11 C12 1.392(9) . ?
C12 C13 1.370(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.375(10) . ?
C13 O1 1.391(8) . ?
C14 C15 1.393(10) . ?
C14 H14 0.9300 . ?
C15 O2 1.390(9) . ?
C15 C16 1.359(10) . ?
C16 H16 0.9300 . ?
C17 O1 1.432(7) . ?
C17 C18 1.516(8) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.538(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.515(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.535(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.527(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.508(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.523(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.518(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.510(4) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.499(5) . ?
C27 O2 1.451(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.526(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.503(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.522(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.513(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.509(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.508(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.511(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.513(5) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
N1 N2 1.361(8) . ?
N1 Pd1 1.929(7) . ?
Pd1 N1 1.929(7) 2_666 ?
Pd1 N3 2.041(7) 2_666 ?
Pd1 N3 2.041(7) . ?
C6 N3 1.328(9) . ?
C6 C7 1.336(10) . ?
C7 C8 1.390(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.382(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.396(10) . ?
C9 H9 0.9300 . ?
C10 N3 1.359(8) . ?
C10 H10 0.9300 . ?

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
N2 C3 C4 106.8(8) . . ?
N2 C3 C11 120.7(9) . . ?
C4 C3 C11 132.5(9) . . ?
C5 C4 C3 108.0(8) . . ?
C5 C4 H4 126.0 . . ?
C3 C4 H4 126.0 . . ?
N1 C5 C4 109.2(9) . . ?
N1 C5 C6 111.6(9) . . ?
C4 C5 C6 139.2(10) . . ?
C16 C11 C12 118.9(9) . . ?
C16 C11 C3 121.1(10) . . ?
C12 C11 C3 119.9(10) . . ?
C11 C12 C13 121.2(9) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C14 C13 C12 120.1(9) . . ?
C14 C13 O1 114.7(9) . . ?
C12 C13 O1 125.1(9) . . ?
C13 C14 C15 117.6(9) . . ?
C13 C14 H14 121.2 . . ?
C15 C14 H14 121.2 . . ?
O2 C15 C16 122.5(10) . . ?
O2 C15 C14 114.9(10) . . ?
C16 C15 C14 122.5(10) . . ?
C15 C16 C11 119.5(10) . . ?
C15 C16 H16 120.2 . . ?
C11 C16 H16 120.2 . . ?
O1 C17 C18 106.6(7) . . ?
O1 C17 H17A 110.4 . . ?
C18 C17 H17A 110.4 . . ?
O1 C17 H17B 110.4 . . ?
C18 C17 H17B 110.4 . . ?
H17A C17 H17B 108.6 . . ?
C17 C18 C19 109.7(7) . . ?
C17 C18 H18A 109.7 . . ?
C19 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
C19 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C20 C19 C18 113.5(7) . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C21 C20 C19 112.7(7) . . ?
C21 C20 H20A 109.1 . . ?
C19 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C20 C21 C22 113.5(7) . . ?
C20 C21 H21A 108.9 . . ?
C22 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
C22 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C23 C22 C21 113.8(7) . . ?
C23 C22 H22A 108.8 . . ?
C21 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
C21 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C22 C23 C24 115.0(7) . . ?
C22 C23 H23A 108.5 . . ?
C24 C23 H23A 108.5 . . ?
C22 C23 H23B 108.5 . . ?
C24 C23 H23B 108.5 . . ?
H23A C23 H23B 107.5 . . ?
C25 C24 C23 111.5(6) . . ?
C25 C24 H24A 109.3 . . ?
C23 C24 H24A 109.3 . . ?
C25 C24 H24B 109.3 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 C26 112.2(7) . . ?
C24 C25 H25A 109.2 . . ?
C26 C25 H25A 109.2 . . ?
C24 C25 H25B 109.2 . . ?
C26 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 O2 112.4(8) . . ?
C28 C27 H27A 109.1 . . ?
O2 C27 H27A 109.1 . . ?
C28 C27 H27B 109.1 . . ?
O2 C27 H27B 109.1 . . ?
H27A C27 H27B 107.9 . . ?
C27 C28 C29 106.8(8) . . ?
C27 C28 H28A 110.4 . . ?
C29 C28 H28A 110.4 . . ?
C27 C28 H28B 110.4 . . ?
C29 C28 H28B 110.4 . . ?
H28A C28 H28B 108.6 . . ?
C30 C29 C28 113.4(7) . . ?
C30 C29 H29A 108.9 . . ?
C28 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C28 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C29 C30 C31 111.4(8) . . ?
C29 C30 H30A 109.4 . . ?
C31 C30 H30A 109.4 . . ?
C29 C30 H30B 109.4 . . ?
C31 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
C32 C31 C30 115.5(7) . . ?
C32 C31 H31A 108.4 . . ?
C30 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
C30 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C31 C32 C33 115.8(8) . . ?
C31 C32 H32A 108.3 . . ?
C33 C32 H32A 108.3 . . ?
C31 C32 H32B 108.3 . . ?
C33 C32 H32B 108.3 . . ?
H32A C32 H32B 107.4 . . ?
C34 C33 C32 117.1(8) . . ?
C34 C33 H33A 108.0 . . ?
C32 C33 H33A 108.0 . . ?
C34 C33 H33B 108.0 . . ?
C32 C33 H33B 108.0 . . ?
H33A C33 H33B 107.3 . . ?
C33 C34 C35 115.9(8) . . ?
C33 C34 H34A 108.3 . . ?
C35 C34 H34A 108.3 . . ?
C33 C34 H34B 108.3 . . ?
C35 C34 H34B 108.3 . . ?
H34A C34 H34B 107.4 . . ?
C36 C35 C34 114.1(9) . . ?
C36 C35 H35A 108.7 . . ?
C34 C35 H35A 108.7 . . ?
C36 C35 H35B 108.7 . . ?
C34 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 N1 C5 106.6(8) . . ?
N2 N1 Pd1 133.7(7) . . ?
C5 N1 Pd1 119.7(7) . . ?
N1 N2 C3 109.4(8) . . ?
C13 O1 C17 116.1(7) . . ?
C15 O2 C27 113.4(8) . . ?
N1 Pd1 N1 180.0(4) . 2_666 ?
N1 Pd1 N3 101.5(4) . 2_666 ?
N1 Pd1 N3 78.5(4) 2_666 2_666 ?
N1 Pd1 N3 78.5(4) . . ?
N1 Pd1 N3 101.5(4) 2_666 . ?
N3 Pd1 N3 180.000(2) 2_666 . ?
N3 C6 C7 121.0(10) . . ?
N3 C6 C5 114.4(11) . . ?
C7 C6 C5 124.6(11) . . ?
C6 C7 C8 122.1(10) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C7 C8 C9 116.6(10) . . ?
C7 C8 H8 121.7 . . ?
C9 C8 H8 121.7 . . ?
C8 C9 C10 120.4(10) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
N3 C10 C9 119.2(9) . . ?
N3 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C6 N3 C10 120.7(9) . . ?
C6 N3 Pd1 115.7(8) . . ?
C10 N3 Pd1 123.5(7) . . ?

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
N2 C3 C4 C5 0.8(9) . . . . ?
C11 C3 C4 C5 -178.6(8) . . . . ?
C3 C4 C5 N1 -0.3(10) . . . . ?
C3 C4 C5 C6 179.4(10) . . . . ?
N2 C3 C11 C16 -2.4(12) . . . . ?
C4 C3 C11 C16 177.0(9) . . . . ?
N2 C3 C11 C12 177.2(7) . . . . ?
C4 C3 C11 C12 -3.4(14) . . . . ?
C16 C11 C12 C13 -1.2(12) . . . . ?
C3 C11 C12 C13 179.2(7) . . . . ?
C11 C12 C13 C14 0.1(12) . . . . ?
C11 C12 C13 O1 177.1(7) . . . . ?
C12 C13 C14 C15 -1.4(13) . . . . ?
O1 C13 C14 C15 -178.7(7) . . . . ?
C13 C14 C15 O2 179.2(7) . . . . ?
C13 C14 C15 C16 4.1(13) . . . . ?
O2 C15 C16 C11 180.0(7) . . . . ?
C14 C15 C16 C11 -5.2(14) . . . . ?
C12 C11 C16 C15 3.6(13) . . . . ?
C3 C11 C16 C15 -176.8(8) . . . . ?
O1 C17 C18 C19 178.6(6) . . . . ?
C17 C18 C19 C20 -179.4(6) . . . . ?
C18 C19 C20 C21 -178.9(6) . . . . ?
C19 C20 C21 C22 -177.7(6) . . . . ?
C20 C21 C22 C23 180.0(7) . . . . ?
C21 C22 C23 C24 177.2(7) . . . . ?
C22 C23 C24 C25 -178.9(7) . . . . ?
C23 C24 C25 C26 178.9(7) . . . . ?
O2 C27 C28 C29 175.6(7) . . . . ?
C27 C28 C29 C30 -175.9(8) . . . . ?
C28 C29 C30 C31 176.5(8) . . . . ?
C29 C30 C31 C32 -179.1(8) . . . . ?
C30 C31 C32 C33 177.1(9) . . . . ?
C31 C32 C33 C34 177.8(9) . . . . ?
C32 C33 C34 C35 -178.8(9) . . . . ?
C33 C34 C35 C36 179.2(9) . . . . ?
C4 C5 N1 N2 -0.4(9) . . . . ?
C6 C5 N1 N2 179.8(7) . . . . ?
C4 C5 N1 Pd1 177.2(5) . . . . ?
C6 C5 N1 Pd1 -2.5(9) . . . . ?
C5 N1 N2 C3 0.9(9) . . . . ?
Pd1 N1 N2 C3 -176.2(6) . . . . ?
C4 C3 N2 N1 -1.1(9) . . . . ?
C11 C3 N2 N1 178.4(7) . . . . ?
C14 C13 O1 C17 179.8(7) . . . . ?
C12 C13 O1 C17 2.6(11) . . . . ?
C18 C17 O1 C13 -177.1(6) . . . . ?
C16 C15 O2 C27 -1.7(13) . . . . ?
C14 C15 O2 C27 -176.9(7) . . . . ?
C28 C27 O2 C15 -177.8(8) . . . . ?
N2 N1 Pd1 N1 93(18) . . . 2_666 ?
C5 N1 Pd1 N1 -84(18) . . . 2_666 ?
N2 N1 Pd1 N3 -0.4(8) . . . 2_666 ?
C5 N1 Pd1 N3 -177.2(6) . . . 2_666 ?
N2 N1 Pd1 N3 179.6(8) . . . . ?
C5 N1 Pd1 N3 2.8(6) . . . . ?
N1 C5 C6 N3 0.3(10) . . . . ?
C4 C5 C6 N3 -179.4(9) . . . . ?
N1 C5 C6 C7 179.8(8) . . . . ?
C4 C5 C6 C7 0.2(17) . . . . ?
N3 C6 C7 C8 -1.8(15) . . . . ?
C5 C6 C7 C8 178.8(8) . . . . ?
C6 C7 C8 C9 2.3(14) . . . . ?
C7 C8 C9 C10 -1.9(14) . . . . ?
C8 C9 C10 N3 1.0(14) . . . . ?
C7 C6 N3 C10 0.7(13) . . . . ?
C5 C6 N3 C10 -179.8(7) . . . . ?
C7 C6 N3 Pd1 -177.6(7) . . . . ?
C5 C6 N3 Pd1 1.9(9) . . . . ?
C9 C10 N3 C6 -0.3(12) . . . . ?
C9 C10 N3 Pd1 177.9(6) . . . . ?
N1 Pd1 N3 C6 -2.5(6) . . . . ?
N1 Pd1 N3 C6 177.5(6) 2_666 . . . ?
N3 Pd1 N3 C6 169(60) 2_666 . . . ?
N1 Pd1 N3 C10 179.2(7) . . . . ?
N1 Pd1 N3 C10 -0.8(7) 2_666 . . . ?
N3 Pd1 N3 C10 -9(60) 2_666 . . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.073


#=======================================================================END   
_database_code_depnum_ccdc_archive 'CCDC 977935'
