Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222

_publ_contact_author             'Andrei S.Batsanov'
_publ_contact_author_email       a.s.batsanov@durham.ac.uk
_journal_volume                  ?
_journal_page_first              ?
_journal_page_last               ?
_database_code_depnum_ccdc_journal ?

_publ_section_title              
; The synthesis, donor properties and coordination chemistry of
chelating N-pyrrolylphosphino-N'-aryl-aldimine ligands
;
_publ_contact_author_name        'Andrei S.Batsanov'
loop_
_publ_author_name
C.E.Anderson
A.S.Batsanov
P.W.Dyer
J.Fawcett
J.A.K.Howard
#============================================================

data_13d
_database_code_depnum_ccdc_archive 'CCDC 617735'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; (2,6-Diisopropyl-phenyl)-(1-diphenylphosphanyl-1H-pyrrol-2-
ylmethylene)-amine palladium dichloride
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H31 Cl2 N2 P Pd'
_chemical_formula_sum            'C29 H31 Cl2 N2 P Pd'
_chemical_formula_weight         615.83

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   32.505(4)
_cell_length_b                   9.9996(11)
_cell_length_c                   17.8876(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.609(2)
_cell_angle_gamma                90.00
_cell_volume                     5673.9(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12694
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      28.61

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2512
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_process_details   
;
absorption correction based on 16940 reflections (SADABS);
Rint 0.039 before correction and 0.025 after.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX 2K CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_reflns_number            21726
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5569
_reflns_number_gt                5187
_reflns_threshold_expression     I>2\s(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 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.
;

_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^)+(0.0388P)^2^+1.2926P] 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         5569
_refine_ls_number_parameters     320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0660
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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 0.151992(4) 0.727074(14) 0.089671(8) 0.01685(6) Uani 1 1 d . . .
Cl1 Cl 0.211401(15) 0.59892(5) 0.12291(3) 0.02567(12) Uani 1 1 d . . .
Cl2 Cl 0.115857(15) 0.55152(5) 0.01615(3) 0.02749(12) Uani 1 1 d . . .
P2 P 0.190396(15) 0.88680(5) 0.15450(3) 0.01761(11) Uani 1 1 d . . .
N1 N 0.09859(5) 0.84418(15) 0.06902(9) 0.0190(3) Uani 1 1 d . . .
N2 N 0.17291(5) 1.03683(15) 0.11342(9) 0.0193(3) Uani 1 1 d . . .
C1 C 0.09693(6) 0.97327(19) 0.06741(11) 0.0227(4) Uani 1 1 d . . .
H1 H 0.0694 1.0107 0.0543 0.027 Uiso 1 1 calc R . .
C2 C 0.13062(6) 1.06706(19) 0.08251(11) 0.0220(4) Uani 1 1 d . . .
C3 C 0.12801(7) 1.2025(2) 0.06822(12) 0.0271(5) Uani 1 1 d . . .
H3 H 0.1030 1.2507 0.0473 0.033 Uiso 1 1 calc R . .
C4 C 0.16861(7) 1.2568(2) 0.08978(12) 0.0269(5) Uani 1 1 d . . .
H4 H 0.1761 1.3479 0.0853 0.032 Uiso 1 1 calc R . .
C5 C 0.19519(6) 1.15582(19) 0.11811(11) 0.0238(4) Uani 1 1 d . . .
H5 H 0.2246 1.1651 0.1381 0.029 Uiso 1 1 calc R . .
C6 C 0.05822(6) 0.77675(18) 0.05402(12) 0.0219(4) Uani 1 1 d . . .
C7 C 0.03307(7) 0.77752(19) -0.02060(13) 0.0268(5) Uani 1 1 d . . .
C8 C -0.00578(7) 0.7138(2) -0.03168(15) 0.0351(5) Uani 1 1 d . . .
H8 H -0.0237 0.7139 -0.0813 0.042 Uiso 1 1 calc R . .
C9 C -0.01886(7) 0.6508(2) 0.02718(16) 0.0413(6) Uani 1 1 d . . .
H9 H -0.0457 0.6086 0.0182 0.050 Uiso 1 1 calc R . .
C10 C 0.00708(7) 0.6489(2) 0.09974(15) 0.0368(5) Uani 1 1 d . . .
H10 H -0.0021 0.6046 0.1401 0.044 Uiso 1 1 calc R . .
C11 C 0.04617(6) 0.7103(2) 0.11455(13) 0.0269(5) Uani 1 1 d . . .
C12 C 0.04721(7) 0.8388(2) -0.08833(12) 0.0345(5) Uani 1 1 d . . .
H12 H 0.0768 0.8717 -0.0701 0.041 Uiso 1 1 calc R . .
C13 C 0.01953(9) 0.9587(3) -0.12017(16) 0.0547(7) Uani 1 1 d . . .
H13A H -0.0097 0.9289 -0.1384 0.082 Uiso 1 1 calc R . .
H13B H 0.0298 0.9982 -0.1628 0.082 Uiso 1 1 calc R . .
H13C H 0.0208 1.0256 -0.0797 0.082 Uiso 1 1 calc R . .
C14 C 0.04722(9) 0.7351(3) -0.15110(15) 0.0531(7) Uani 1 1 d . . .
H14A H 0.0650 0.6593 -0.1297 0.080 Uiso 1 1 calc R . .
H14B H 0.0583 0.7758 -0.1925 0.080 Uiso 1 1 calc R . .
H14C H 0.0184 0.7039 -0.1713 0.080 Uiso 1 1 calc R . .
C15 C 0.07473(7) 0.7068(2) 0.19409(13) 0.0343(5) Uani 1 1 d . . .
H15 H 0.1044 0.7137 0.1876 0.041 Uiso 1 1 calc R . .
C16 C 0.06672(9) 0.8262(3) 0.24093(14) 0.0571(8) Uani 1 1 d . . .
H16A H 0.0711 0.9088 0.2142 0.086 Uiso 1 1 calc R . .
H16B H 0.0862 0.8239 0.2911 0.086 Uiso 1 1 calc R . .
H16C H 0.0376 0.8233 0.2478 0.086 Uiso 1 1 calc R . .
C17 C 0.07120(9) 0.5768(3) 0.23681(18) 0.0649(9) Uani 1 1 d . . .
H17A H 0.0427 0.5688 0.2463 0.097 Uiso 1 1 calc R . .
H17B H 0.0918 0.5771 0.2858 0.097 Uiso 1 1 calc R . .
H17C H 0.0768 0.5009 0.2058 0.097 Uiso 1 1 calc R . .
C18 C 0.18530(6) 0.89878(19) 0.25291(11) 0.0213(4) Uani 1 1 d . . .
C19 C 0.17965(7) 1.0209(2) 0.28632(12) 0.0298(5) Uani 1 1 d . . .
H19 H 0.1787 1.1013 0.2577 0.036 Uiso 1 1 calc R . .
C20 C 0.17543(8) 1.0244(2) 0.36172(13) 0.0385(6) Uani 1 1 d . . .
H20 H 0.1716 1.1077 0.3848 0.046 Uiso 1 1 calc R . .
C21 C 0.17679(8) 0.9085(2) 0.40351(13) 0.0392(6) Uani 1 1 d . . .
H21 H 0.1739 0.9121 0.4552 0.047 Uiso 1 1 calc R . .
C22 C 0.18232(8) 0.7871(2) 0.37048(13) 0.0364(6) Uani 1 1 d . . .
H22 H 0.1832 0.7071 0.3995 0.044 Uiso 1 1 calc R . .
C23 C 0.18653(7) 0.7815(2) 0.29523(12) 0.0284(5) Uani 1 1 d . . .
H23 H 0.1903 0.6978 0.2725 0.034 Uiso 1 1 calc R . .
C24 C 0.24552(6) 0.89456(18) 0.15327(11) 0.0200(4) Uani 1 1 d . . .
C25 C 0.27600(6) 0.89570(19) 0.22053(11) 0.0241(4) Uani 1 1 d . . .
H25 H 0.2681 0.8924 0.2685 0.029 Uiso 1 1 calc R . .
C26 C 0.31840(6) 0.9017(2) 0.21759(13) 0.0300(5) Uani 1 1 d . . .
H26 H 0.3395 0.9023 0.2636 0.036 Uiso 1 1 calc R . .
C27 C 0.32962(7) 0.9068(2) 0.14791(13) 0.0306(5) Uani 1 1 d . . .
H27 H 0.3586 0.9107 0.1460 0.037 Uiso 1 1 calc R . .
C28 C 0.29907(7) 0.9063(2) 0.08029(12) 0.0311(5) Uani 1 1 d . . .
H28 H 0.3071 0.9109 0.0324 0.037 Uiso 1 1 calc R . .
C29 C 0.25725(7) 0.8991(2) 0.08282(12) 0.0273(5) Uani 1 1 d . . .
H29 H 0.2363 0.8972 0.0366 0.033 Uiso 1 1 calc R . .

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 0.01460(9) 0.01539(9) 0.02007(9) -0.00009(5) 0.00267(6) -0.00048(5)
Cl1 0.0208(2) 0.0192(2) 0.0338(3) 0.00092(19) -0.0010(2) 0.00363(18)
Cl2 0.0185(2) 0.0205(2) 0.0417(3) -0.0075(2) 0.0028(2) -0.00240(18)
P2 0.0169(2) 0.0169(2) 0.0182(2) 0.00040(18) 0.00214(18) -0.00033(19)
N1 0.0153(8) 0.0183(8) 0.0228(8) -0.0005(6) 0.0028(6) 0.0008(6)
N2 0.0182(8) 0.0171(8) 0.0214(8) 0.0008(6) 0.0018(6) -0.0006(6)
C1 0.0177(10) 0.0252(10) 0.0244(10) 0.0012(8) 0.0031(8) 0.0030(8)
C2 0.0208(10) 0.0210(10) 0.0235(10) 0.0001(8) 0.0032(8) 0.0023(8)
C3 0.0276(12) 0.0206(10) 0.0318(11) 0.0014(9) 0.0034(9) 0.0034(9)
C4 0.0326(12) 0.0180(10) 0.0293(12) 0.0000(8) 0.0048(9) -0.0043(9)
C5 0.0238(10) 0.0203(10) 0.0260(10) -0.0010(8) 0.0022(8) -0.0064(8)
C6 0.0149(10) 0.0186(10) 0.0326(11) -0.0024(8) 0.0059(8) 0.0013(7)
C7 0.0201(11) 0.0238(11) 0.0344(12) -0.0040(8) 0.0014(9) 0.0030(8)
C8 0.0213(11) 0.0310(12) 0.0476(14) -0.0079(10) -0.0041(10) 0.0023(9)
C9 0.0202(11) 0.0274(12) 0.0749(18) -0.0004(12) 0.0076(11) -0.0040(9)
C10 0.0238(11) 0.0297(12) 0.0598(16) 0.0100(11) 0.0156(11) 0.0008(9)
C11 0.0191(10) 0.0233(10) 0.0395(12) 0.0039(9) 0.0092(9) 0.0046(8)
C12 0.0285(12) 0.0450(14) 0.0274(11) -0.0006(10) 0.0007(9) 0.0010(10)
C13 0.0610(18) 0.0528(17) 0.0507(16) 0.0173(13) 0.0131(14) 0.0094(14)
C14 0.0511(18) 0.071(2) 0.0343(15) -0.0092(13) 0.0031(13) 0.0131(14)
C15 0.0239(12) 0.0434(14) 0.0382(13) 0.0134(10) 0.0123(10) 0.0052(10)
C16 0.0533(17) 0.082(2) 0.0341(14) -0.0044(14) 0.0055(12) 0.0260(16)
C17 0.0493(17) 0.071(2) 0.074(2) 0.0428(17) 0.0107(15) 0.0056(15)
C18 0.0190(10) 0.0254(10) 0.0189(9) -0.0006(8) 0.0029(7) -0.0017(8)
C19 0.0394(13) 0.0237(11) 0.0280(11) -0.0016(9) 0.0112(9) -0.0048(9)
C20 0.0533(15) 0.0343(13) 0.0306(12) -0.0110(10) 0.0148(11) -0.0056(11)
C21 0.0495(15) 0.0473(15) 0.0229(11) -0.0023(10) 0.0127(10) -0.0055(12)
C22 0.0488(15) 0.0328(13) 0.0274(12) 0.0076(9) 0.0080(11) 0.0002(11)
C23 0.0326(12) 0.0252(11) 0.0273(11) 0.0023(8) 0.0060(9) 0.0026(9)
C24 0.0179(9) 0.0179(9) 0.0237(10) -0.0010(7) 0.0035(8) 0.0000(7)
C25 0.0239(10) 0.0240(10) 0.0235(10) -0.0010(8) 0.0031(8) -0.0013(8)
C26 0.0205(11) 0.0319(12) 0.0333(12) -0.0004(9) -0.0033(9) -0.0013(9)
C27 0.0187(10) 0.0311(12) 0.0428(13) -0.0041(10) 0.0087(9) -0.0014(9)
C28 0.0303(12) 0.0365(12) 0.0293(11) -0.0029(9) 0.0122(9) -0.0031(9)
C29 0.0249(11) 0.0332(12) 0.0227(10) -0.0011(9) 0.0026(8) -0.0023(9)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 2.0593(15) . ?
Pd1 P2 2.1959(5) . ?
Pd1 Cl1 2.2855(5) . ?
Pd1 Cl2 2.3487(5) . ?
P2 N2 1.7121(16) . ?
P2 C24 1.7983(19) . ?
P2 C18 1.8078(19) . ?
N1 C1 1.292(2) . ?
N1 C6 1.447(2) . ?
N2 C5 1.386(2) . ?
N2 C2 1.398(2) . ?
C1 C2 1.422(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.377(3) . ?
C3 C4 1.401(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.354(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C11 1.397(3) . ?
C6 C7 1.405(3) . ?
C7 C8 1.389(3) . ?
C7 C12 1.516(3) . ?
C8 C9 1.372(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 C15 1.520(3) . ?
C12 C14 1.528(3) . ?
C12 C13 1.532(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.513(4) . ?
C15 C17 1.526(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.389(3) . ?
C18 C23 1.392(3) . ?
C19 C20 1.385(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.375(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.384(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.382(3) . ?
C24 C29 1.395(3) . ?
C25 C26 1.392(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.374(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.372(3) . ?
C28 H28 0.9500 . ?
C29 H29 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
N1 Pd1 P2 92.34(4) . . ?
N1 Pd1 Cl1 175.38(4) . . ?
P2 Pd1 Cl1 85.402(19) . . ?
N1 Pd1 Cl2 91.47(4) . . ?
P2 Pd1 Cl2 175.189(18) . . ?
Cl1 Pd1 Cl2 90.998(18) . . ?
N2 P2 C24 101.26(8) . . ?
N2 P2 C18 105.51(8) . . ?
C24 P2 C18 108.21(9) . . ?
N2 P2 Pd1 108.27(6) . . ?
C24 P2 Pd1 118.55(6) . . ?
C18 P2 Pd1 113.58(6) . . ?
C1 N1 C6 115.45(16) . . ?
C1 N1 Pd1 126.98(13) . . ?
C6 N1 Pd1 117.58(11) . . ?
C5 N2 C2 107.10(15) . . ?
C5 N2 P2 127.31(13) . . ?
C2 N2 P2 124.39(13) . . ?
N1 C1 C2 128.90(18) . . ?
N1 C1 H1 115.5 . . ?
C2 C1 H1 115.5 . . ?
C3 C2 N2 107.55(17) . . ?
C3 C2 C1 126.82(19) . . ?
N2 C2 C1 125.62(17) . . ?
C2 C3 C4 108.32(19) . . ?
C2 C3 H3 125.8 . . ?
C4 C3 H3 125.8 . . ?
C5 C4 C3 107.41(18) . . ?
C5 C4 H4 126.3 . . ?
C3 C4 H4 126.3 . . ?
C4 C5 N2 109.61(18) . . ?
C4 C5 H5 125.2 . . ?
N2 C5 H5 125.2 . . ?
C11 C6 C7 122.36(19) . . ?
C11 C6 N1 118.31(18) . . ?
C7 C6 N1 119.31(18) . . ?
C8 C7 C6 117.1(2) . . ?
C8 C7 C12 119.7(2) . . ?
C6 C7 C12 123.14(19) . . ?
C9 C8 C7 121.7(2) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C10 119.9(2) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C9 C10 C11 121.3(2) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 117.6(2) . . ?
C10 C11 C15 121.1(2) . . ?
C6 C11 C15 121.24(19) . . ?
C7 C12 C14 111.2(2) . . ?
C7 C12 C13 110.95(19) . . ?
C14 C12 C13 110.6(2) . . ?
C7 C12 H12 108.0 . . ?
C14 C12 H12 108.0 . . ?
C13 C12 H12 108.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C16 110.89(19) . . ?
C11 C15 C17 113.0(2) . . ?
C16 C15 C17 110.8(2) . . ?
C11 C15 H15 107.3 . . ?
C16 C15 H15 107.3 . . ?
C17 C15 H15 107.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 119.85(18) . . ?
C19 C18 P2 121.73(15) . . ?
C23 C18 P2 118.41(15) . . ?
C18 C19 C20 119.4(2) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C21 C20 C19 120.7(2) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 120.1(2) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C23 120.1(2) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C18 119.86(19) . . ?
C22 C23 H23 120.1 . . ?
C18 C23 H23 120.1 . . ?
C25 C24 C29 120.06(18) . . ?
C25 C24 P2 121.11(15) . . ?
C29 C24 P2 118.82(15) . . ?
C24 C25 C26 119.69(19) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C27 C26 C25 119.8(2) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C26 C27 C28 120.6(2) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C29 C28 C27 119.8(2) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C24 119.99(19) . . ?
C28 C29 H29 120.0 . . ?
C24 C29 H29 120.0 . . ?

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
N1 Pd1 P2 N2 -35.13(7) . . . . ?
Cl1 Pd1 P2 N2 148.91(6) . . . . ?
N1 Pd1 P2 C24 -149.57(8) . . . . ?
Cl1 Pd1 P2 C24 34.47(7) . . . . ?
N1 Pd1 P2 C18 81.70(8) . . . . ?
Cl1 Pd1 P2 C18 -94.26(7) . . . . ?
P2 Pd1 N1 C1 25.00(16) . . . . ?
Cl2 Pd1 N1 C1 -152.06(16) . . . . ?
P2 Pd1 N1 C6 -155.46(13) . . . . ?
Cl2 Pd1 N1 C6 27.47(13) . . . . ?
C24 P2 N2 C5 -31.72(18) . . . . ?
C18 P2 N2 C5 80.98(17) . . . . ?
Pd1 P2 N2 C5 -157.10(15) . . . . ?
C24 P2 N2 C2 162.46(16) . . . . ?
C18 P2 N2 C2 -84.84(17) . . . . ?
Pd1 P2 N2 C2 37.09(16) . . . . ?
C6 N1 C1 C2 177.33(19) . . . . ?
Pd1 N1 C1 C2 -3.1(3) . . . . ?
C5 N2 C2 C3 0.7(2) . . . . ?
P2 N2 C2 C3 168.93(14) . . . . ?
C5 N2 C2 C1 179.47(18) . . . . ?
P2 N2 C2 C1 -12.3(3) . . . . ?
N1 C1 C2 C3 168.6(2) . . . . ?
N1 C1 C2 N2 -9.9(3) . . . . ?
N2 C2 C3 C4 0.3(2) . . . . ?
C1 C2 C3 C4 -178.5(2) . . . . ?
C2 C3 C4 C5 -1.2(3) . . . . ?
C3 C4 C5 N2 1.6(2) . . . . ?
C2 N2 C5 C4 -1.5(2) . . . . ?
P2 N2 C5 C4 -169.24(15) . . . . ?
C1 N1 C6 C11 -109.9(2) . . . . ?
Pd1 N1 C6 C11 70.5(2) . . . . ?
C1 N1 C6 C7 71.5(2) . . . . ?
Pd1 N1 C6 C7 -108.08(17) . . . . ?
C11 C6 C7 C8 2.8(3) . . . . ?
N1 C6 C7 C8 -178.67(17) . . . . ?
C11 C6 C7 C12 -174.61(19) . . . . ?
N1 C6 C7 C12 3.9(3) . . . . ?
C6 C7 C8 C9 -1.1(3) . . . . ?
C12 C7 C8 C9 176.5(2) . . . . ?
C7 C8 C9 C10 -0.5(3) . . . . ?
C8 C9 C10 C11 0.4(4) . . . . ?
C9 C10 C11 C6 1.3(3) . . . . ?
C9 C10 C11 C15 -179.4(2) . . . . ?
C7 C6 C11 C10 -2.9(3) . . . . ?
N1 C6 C11 C10 178.55(18) . . . . ?
C7 C6 C11 C15 177.74(19) . . . . ?
N1 C6 C11 C15 -0.8(3) . . . . ?
C8 C7 C12 C14 -56.3(3) . . . . ?
C6 C7 C12 C14 121.1(2) . . . . ?
C8 C7 C12 C13 67.3(3) . . . . ?
C6 C7 C12 C13 -115.3(2) . . . . ?
C10 C11 C15 C16 -90.7(3) . . . . ?
C6 C11 C15 C16 88.6(3) . . . . ?
C10 C11 C15 C17 34.3(3) . . . . ?
C6 C11 C15 C17 -146.4(2) . . . . ?
N2 P2 C18 C19 -15.70(19) . . . . ?
C24 P2 C18 C19 92.03(18) . . . . ?
Pd1 P2 C18 C19 -134.13(16) . . . . ?
N2 P2 C18 C23 163.37(16) . . . . ?
C24 P2 C18 C23 -88.90(18) . . . . ?
Pd1 P2 C18 C23 44.94(18) . . . . ?
C23 C18 C19 C20 0.2(3) . . . . ?
P2 C18 C19 C20 179.28(17) . . . . ?
C18 C19 C20 C21 0.0(4) . . . . ?
C19 C20 C21 C22 -0.1(4) . . . . ?
C20 C21 C22 C23 0.0(4) . . . . ?
C21 C22 C23 C18 0.2(4) . . . . ?
C19 C18 C23 C22 -0.3(3) . . . . ?
P2 C18 C23 C22 -179.40(18) . . . . ?
N2 P2 C24 C25 116.40(16) . . . . ?
C18 P2 C24 C25 5.76(18) . . . . ?
Pd1 P2 C24 C25 -125.42(14) . . . . ?
N2 P2 C24 C29 -63.76(17) . . . . ?
C18 P2 C24 C29 -174.41(15) . . . . ?
Pd1 P2 C24 C29 54.42(17) . . . . ?
C29 C24 C25 C26 0.1(3) . . . . ?
P2 C24 C25 C26 179.98(15) . . . . ?
C24 C25 C26 C27 0.2(3) . . . . ?
C25 C26 C27 C28 0.1(3) . . . . ?
C26 C27 C28 C29 -0.8(3) . . . . ?
C27 C28 C29 C24 1.1(3) . . . . ?
C25 C24 C29 C28 -0.8(3) . . . . ?
P2 C24 C29 C28 179.41(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.066

#============================================END

data_14b
_database_code_depnum_ccdc_archive 'CCDC 617736'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; (3,5-Dimethyl-phenyl)-(bis-(diisopropyl)aminophosphanyl)-
(1H-pyrrol-2-ylmethylene)-amine palladium dichloride,
dichloromethane disolvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C25 H41 Cl2 N4 P Pd),2(C H2 Cl2)'
_chemical_formula_sum            'C27 H45 Cl6 N4 P Pd'
_chemical_formula_weight         775.74

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'
P P 0.1023 0.0942 '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'

_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                   13.742(3)
_cell_length_b                   17.691(4)
_cell_length_c                   14.077(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.965(4)
_cell_angle_gamma                90.00
_cell_volume                     3420.5(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4464
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      25.33

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1592
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_process_details   
;
absorption correction based on 9366 reflections (SADABS);
R(int) 0.068 before correction and 0.044 after.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX 2K 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            26447
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6713
_reflns_number_gt                5165
_reflns_threshold_expression     I>2s\(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 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.
;

_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^)+(0.0378P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6713
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.006
_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 0.84215(2) 0.827243(16) 0.24257(2) 0.01931(9) Uani 1 1 d . . .
P1 P 0.76426(7) 0.93122(6) 0.19808(7) 0.0198(2) Uani 1 1 d . . .
Cl1 Cl 0.79021(9) 0.84411(7) 0.39302(7) 0.0393(3) Uani 1 1 d . . .
Cl2 Cl 0.91056(7) 0.71073(5) 0.28927(7) 0.0274(2) Uani 1 1 d . . .
N1 N 0.7185(2) 0.91370(17) 0.0852(2) 0.0200(7) Uani 1 1 d . . .
N2 N 0.8972(2) 0.81483(16) 0.1109(2) 0.0194(7) Uani 1 1 d . . .
N3 N 0.6628(2) 0.95915(18) 0.2480(2) 0.0229(7) Uani 1 1 d . . .
N4 N 0.8382(2) 1.00266(17) 0.1882(2) 0.0220(7) Uani 1 1 d . . .
C1 C 0.6418(3) 0.9490(2) 0.0393(3) 0.0281(10) Uani 1 1 d . . .
H1 H 0.5977 0.9827 0.0681 0.034 Uiso 1 1 calc R . .
C2 C 0.6385(3) 0.9286(2) -0.0538(3) 0.0316(10) Uani 1 1 d . . .
H2 H 0.5920 0.9449 -0.1010 0.038 Uiso 1 1 calc R . .
C3 C 0.7155(3) 0.8794(2) -0.0672(3) 0.0305(10) Uani 1 1 d . . .
H3 H 0.7311 0.8562 -0.1255 0.037 Uiso 1 1 calc R . .
C4 C 0.7648(3) 0.8702(2) 0.0173(3) 0.0218(9) Uani 1 1 d . . .
C5 C 0.8529(3) 0.8303(2) 0.0321(3) 0.0242(9) Uani 1 1 d . . .
H5 H 0.8831 0.8128 -0.0235 0.029 Uiso 1 1 calc R . .
C6 C 0.9929(3) 0.7822(2) 0.1030(3) 0.0212(9) Uani 1 1 d . . .
C7 C 1.0080(3) 0.7269(2) 0.0357(3) 0.0248(9) Uani 1 1 d . . .
H7 H 0.9547 0.7074 -0.0015 0.030 Uiso 1 1 calc R . .
C8 C 1.1011(3) 0.7002(2) 0.0230(3) 0.0262(9) Uani 1 1 d . . .
C9 C 1.1765(3) 0.7292(2) 0.0782(3) 0.0272(10) Uani 1 1 d . . .
H9 H 1.2408 0.7115 0.0689 0.033 Uiso 1 1 calc R . .
C10 C 1.1616(3) 0.7835(2) 0.1468(3) 0.0252(9) Uani 1 1 d . . .
C11 C 1.0686(3) 0.8095(2) 0.1589(3) 0.0214(9) Uani 1 1 d . . .
H11 H 1.0568 0.8464 0.2061 0.026 Uiso 1 1 calc R . .
C12 C 1.1175(3) 0.6413(3) -0.0513(3) 0.0411(12) Uani 1 1 d . . .
H12A H 1.1872 0.6298 -0.0532 0.062 Uiso 1 1 calc R . .
H12B H 1.0944 0.6602 -0.1134 0.062 Uiso 1 1 calc R . .
H12C H 1.0817 0.5952 -0.0357 0.062 Uiso 1 1 calc R . .
C13 C 1.2452(3) 0.8152(2) 0.2047(3) 0.0337(11) Uani 1 1 d . . .
H13A H 1.2582 0.8670 0.1840 0.051 Uiso 1 1 calc R . .
H13B H 1.3032 0.7840 0.1961 0.051 Uiso 1 1 calc R . .
H13C H 1.2292 0.8154 0.2720 0.051 Uiso 1 1 calc R . .
C14 C 0.8071(3) 1.0680(2) 0.1281(3) 0.0259(9) Uani 1 1 d . . .
H14 H 0.7345 1.0644 0.1215 0.031 Uiso 1 1 calc R . .
C15 C 0.8435(3) 1.0641(2) 0.0280(3) 0.0354(11) Uani 1 1 d . . .
H15A H 0.9130 1.0764 0.0288 0.053 Uiso 1 1 calc R . .
H15B H 0.8075 1.1004 -0.0123 0.053 Uiso 1 1 calc R . .
H15C H 0.8335 1.0130 0.0028 0.053 Uiso 1 1 calc R . .
C16 C 0.8281(3) 1.1445(2) 0.1712(3) 0.0345(11) Uani 1 1 d . . .
H16A H 0.7956 1.1487 0.2319 0.052 Uiso 1 1 calc R . .
H16B H 0.8038 1.1840 0.1278 0.052 Uiso 1 1 calc R . .
H16C H 0.8985 1.1504 0.1820 0.052 Uiso 1 1 calc R . .
C17 C 0.9367(3) 0.9973(2) 0.2353(3) 0.0283(10) Uani 1 1 d . . .
H17 H 0.9446 0.9433 0.2551 0.034 Uiso 1 1 calc R . .
C18 C 1.0175(3) 1.0128(3) 0.1678(3) 0.0392(12) Uani 1 1 d . . .
H18A H 1.0081 0.9814 0.1108 0.059 Uiso 1 1 calc R . .
H18B H 1.0804 1.0006 0.1990 0.059 Uiso 1 1 calc R . .
H18C H 1.0164 1.0663 0.1497 0.059 Uiso 1 1 calc R . .
C19 C 0.9474(3) 1.0432(3) 0.3254(3) 0.0412(12) Uani 1 1 d . . .
H19A H 0.9494 1.0970 0.3094 0.062 Uiso 1 1 calc R . .
H19B H 1.0078 1.0289 0.3598 0.062 Uiso 1 1 calc R . .
H19C H 0.8919 1.0334 0.3655 0.062 Uiso 1 1 calc R . .
C20 C 0.6672(3) 1.0277(2) 0.3108(3) 0.0287(10) Uani 1 1 d . . .
H20 H 0.7359 1.0463 0.3097 0.034 Uiso 1 1 calc R . .
C21 C 0.6476(4) 1.0121(3) 0.4135(3) 0.0422(12) Uani 1 1 d . . .
H21A H 0.5787 0.9992 0.4196 0.063 Uiso 1 1 calc R . .
H21B H 0.6630 1.0571 0.4515 0.063 Uiso 1 1 calc R . .
H21C H 0.6881 0.9698 0.4361 0.063 Uiso 1 1 calc R . .
C22 C 0.6036(3) 1.0923(2) 0.2727(3) 0.0390(12) Uani 1 1 d . . .
H22A H 0.6110 1.0971 0.2040 0.058 Uiso 1 1 calc R . .
H22B H 0.6236 1.1396 0.3040 0.058 Uiso 1 1 calc R . .
H22C H 0.5353 1.0819 0.2857 0.058 Uiso 1 1 calc R . .
C23 C 0.5853(3) 0.9029(2) 0.2702(3) 0.0281(10) Uani 1 1 d . . .
H23 H 0.5920 0.8915 0.3397 0.034 Uiso 1 1 calc R . .
C25 C 0.5908(3) 0.8286(2) 0.2180(3) 0.0349(11) Uani 1 1 d . . .
H25A H 0.5809 0.8373 0.1496 0.052 Uiso 1 1 calc R . .
H25B H 0.5401 0.7945 0.2401 0.052 Uiso 1 1 calc R . .
H25C H 0.6549 0.8057 0.2304 0.052 Uiso 1 1 calc R . .
C24 C 0.4847(3) 0.9360(3) 0.2521(4) 0.0449(13) Uani 1 1 d . . .
H24A H 0.4746 0.9778 0.2964 0.067 Uiso 1 1 calc R . .
H24B H 0.4355 0.8969 0.2617 0.067 Uiso 1 1 calc R . .
H24C H 0.4788 0.9548 0.1867 0.067 Uiso 1 1 calc R . .
C27 C 0.7628(4) 0.6036(3) 0.1314(3) 0.0486(13) Uani 1 1 d . . .
H27A H 0.8107 0.6304 0.1734 0.058 Uiso 1 1 calc R . .
H27B H 0.7881 0.6027 0.0664 0.058 Uiso 1 1 calc R . .
C26 C 0.5148(4) 0.2271(3) 0.0475(5) 0.0716(18) Uani 1 1 d . . .
H26A H 0.4540 0.2287 0.0079 0.086 Uiso 1 1 calc R . .
H26B H 0.4975 0.2138 0.1132 0.086 Uiso 1 1 calc R . .
Cl3 Cl 0.59147(10) 0.15690(8) 0.00368(10) 0.0561(4) Uani 1 1 d . . .
Cl4 Cl 0.56805(14) 0.31454(10) 0.04790(15) 0.0986(7) Uani 1 1 d . . .
Cl5 Cl 0.74814(11) 0.51142(8) 0.17181(11) 0.0624(4) Uani 1 1 d . . .
Cl6 Cl 0.65365(15) 0.65092(10) 0.13047(16) 0.1070(7) Uani 1 1 d . . .

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 0.02330(17) 0.01859(16) 0.01619(16) 0.00107(13) 0.00270(12) 0.00346(13)
P1 0.0223(6) 0.0187(5) 0.0187(5) 0.0007(4) 0.0028(4) 0.0028(4)
Cl1 0.0500(7) 0.0485(7) 0.0199(5) 0.0036(5) 0.0084(5) 0.0242(6)
Cl2 0.0344(6) 0.0232(5) 0.0249(5) 0.0063(4) 0.0062(5) 0.0083(4)
N1 0.0217(18) 0.0196(17) 0.0188(18) 0.0008(13) 0.0023(14) 0.0032(14)
N2 0.0233(18) 0.0188(17) 0.0161(17) -0.0005(13) 0.0005(14) 0.0002(14)
N3 0.0232(18) 0.0231(17) 0.0225(18) 0.0007(14) 0.0041(14) 0.0038(15)
N4 0.0244(18) 0.0178(17) 0.0240(18) -0.0004(14) 0.0029(15) 0.0004(14)
C1 0.027(2) 0.027(2) 0.030(2) 0.0043(19) -0.0018(19) 0.0082(19)
C2 0.033(3) 0.036(3) 0.025(2) 0.007(2) -0.009(2) 0.006(2)
C3 0.037(3) 0.034(2) 0.021(2) -0.0022(19) 0.001(2) 0.002(2)
C4 0.027(2) 0.021(2) 0.018(2) -0.0002(16) -0.0015(17) 0.0027(17)
C5 0.028(2) 0.018(2) 0.026(2) -0.0029(18) 0.0060(18) -0.0005(18)
C6 0.025(2) 0.021(2) 0.018(2) 0.0045(16) 0.0102(17) 0.0040(17)
C7 0.028(2) 0.022(2) 0.024(2) -0.0007(17) 0.0019(18) 0.0037(18)
C8 0.034(2) 0.024(2) 0.020(2) 0.0011(17) 0.0061(19) 0.0068(19)
C9 0.023(2) 0.033(2) 0.026(2) 0.0039(19) 0.0061(18) 0.0088(19)
C10 0.024(2) 0.026(2) 0.025(2) 0.0080(18) 0.0040(18) -0.0032(18)
C11 0.027(2) 0.019(2) 0.018(2) 0.0002(16) 0.0028(17) 0.0007(17)
C12 0.048(3) 0.042(3) 0.034(3) -0.007(2) 0.010(2) 0.015(2)
C13 0.027(2) 0.036(3) 0.038(3) 0.002(2) 0.002(2) -0.002(2)
C14 0.028(2) 0.017(2) 0.032(2) 0.0036(17) 0.0041(19) -0.0012(18)
C15 0.048(3) 0.027(2) 0.032(3) 0.0049(19) 0.011(2) -0.004(2)
C16 0.038(3) 0.019(2) 0.046(3) -0.001(2) 0.003(2) -0.0001(19)
C17 0.023(2) 0.023(2) 0.038(3) -0.0048(19) 0.0000(19) -0.0001(18)
C18 0.026(2) 0.034(3) 0.058(3) -0.008(2) 0.007(2) -0.006(2)
C19 0.040(3) 0.047(3) 0.036(3) -0.013(2) -0.007(2) 0.002(2)
C20 0.031(2) 0.023(2) 0.033(3) -0.0060(19) 0.008(2) 0.0051(19)
C21 0.054(3) 0.043(3) 0.030(3) -0.009(2) 0.007(2) 0.020(2)
C22 0.045(3) 0.032(3) 0.040(3) -0.002(2) 0.010(2) 0.010(2)
C23 0.023(2) 0.031(2) 0.030(2) 0.0054(19) 0.0059(19) 0.0002(19)
C25 0.033(3) 0.032(2) 0.040(3) 0.001(2) 0.005(2) -0.009(2)
C24 0.027(3) 0.046(3) 0.061(3) 0.011(3) 0.009(2) 0.002(2)
C27 0.055(3) 0.054(3) 0.038(3) -0.004(2) 0.006(3) -0.016(3)
C26 0.067(4) 0.061(4) 0.088(5) -0.011(3) 0.021(4) -0.004(3)
Cl3 0.0522(8) 0.0563(9) 0.0597(9) 0.0024(7) 0.0013(7) 0.0045(7)
Cl4 0.0964(14) 0.0636(11) 0.1401(18) -0.0277(11) 0.0658(13) -0.0221(10)
Cl5 0.0607(9) 0.0517(9) 0.0745(10) 0.0086(7) -0.0037(8) -0.0033(7)
Cl6 0.1120(16) 0.0678(12) 0.1433(19) 0.0106(12) 0.0319(14) 0.0440(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 N2 2.037(3) . ?
Pd1 P1 2.2081(11) . ?
Pd1 Cl1 2.2776(11) . ?
Pd1 Cl2 2.3499(10) . ?
P1 N4 1.631(3) . ?
P1 N3 1.658(3) . ?
P1 N1 1.717(3) . ?
N1 C1 1.368(5) . ?
N1 C4 1.398(5) . ?
N2 C5 1.277(5) . ?
N2 C6 1.444(5) . ?
N3 C23 1.498(5) . ?
N3 C20 1.500(5) . ?
N4 C14 1.487(5) . ?
N4 C17 1.489(5) . ?
C1 C2 1.359(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.388(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.358(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(5) . ?
C5 H5 0.9500 . ?
C6 C11 1.370(5) . ?
C6 C7 1.383(5) . ?
C7 C8 1.382(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.373(6) . ?
C8 C12 1.499(5) . ?
C9 C10 1.383(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.374(5) . ?
C10 C13 1.495(5) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.507(5) . ?
C14 C15 1.513(5) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.508(5) . ?
C17 C18 1.512(6) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.504(6) . ?
C20 C22 1.526(6) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.511(6) . ?
C23 C24 1.515(5) . ?
C23 H23 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C27 Cl6 1.717(5) . ?
C27 Cl5 1.741(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C26 Cl4 1.711(6) . ?
C26 Cl3 1.754(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?

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 Pd1 P1 91.33(9) . . ?
N2 Pd1 Cl1 176.29(9) . . ?
P1 Pd1 Cl1 89.44(4) . . ?
N2 Pd1 Cl2 90.15(9) . . ?
P1 Pd1 Cl2 174.53(4) . . ?
Cl1 Pd1 Cl2 89.42(4) . . ?
N4 P1 N3 109.91(17) . . ?
N4 P1 N1 105.72(16) . . ?
N3 P1 N1 99.19(16) . . ?
N4 P1 Pd1 111.85(12) . . ?
N3 P1 Pd1 122.31(12) . . ?
N1 P1 Pd1 105.70(11) . . ?
C1 N1 C4 106.9(3) . . ?
C1 N1 P1 127.3(3) . . ?
C4 N1 P1 124.9(3) . . ?
C5 N2 C6 115.2(3) . . ?
C5 N2 Pd1 126.0(3) . . ?
C6 N2 Pd1 118.7(2) . . ?
C23 N3 C20 115.4(3) . . ?
C23 N3 P1 120.3(3) . . ?
C20 N3 P1 118.2(3) . . ?
C14 N4 C17 122.9(3) . . ?
C14 N4 P1 118.9(3) . . ?
C17 N4 P1 118.2(3) . . ?
C2 C1 N1 109.5(4) . . ?
C2 C1 H1 125.2 . . ?
N1 C1 H1 125.2 . . ?
C1 C2 C3 107.3(4) . . ?
C1 C2 H2 126.4 . . ?
C3 C2 H2 126.4 . . ?
C4 C3 C2 108.5(4) . . ?
C4 C3 H3 125.8 . . ?
C2 C3 H3 125.8 . . ?
C3 C4 N1 107.9(3) . . ?
C3 C4 C5 126.1(4) . . ?
N1 C4 C5 125.7(3) . . ?
N2 C5 C4 128.0(4) . . ?
N2 C5 H5 116.0 . . ?
C4 C5 H5 116.0 . . ?
C11 C6 C7 120.9(4) . . ?
C11 C6 N2 119.4(3) . . ?
C7 C6 N2 119.6(4) . . ?
C8 C7 C6 119.5(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C9 C8 C7 118.9(4) . . ?
C9 C8 C12 121.7(4) . . ?
C7 C8 C12 119.4(4) . . ?
C8 C9 C10 121.9(4) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C11 C10 C9 118.6(4) . . ?
C11 C10 C13 120.6(4) . . ?
C9 C10 C13 120.8(4) . . ?
C6 C11 C10 120.2(4) . . ?
C6 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C14 C16 114.9(3) . . ?
N4 C14 C15 113.4(3) . . ?
C16 C14 C15 110.5(3) . . ?
N4 C14 H14 105.7 . . ?
C16 C14 H14 105.7 . . ?
C15 C14 H14 105.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C19 113.6(3) . . ?
N4 C17 C18 112.6(3) . . ?
C19 C17 C18 112.2(4) . . ?
N4 C17 H17 105.9 . . ?
C19 C17 H17 105.9 . . ?
C18 C17 H17 105.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 C21 114.4(3) . . ?
N3 C20 C22 112.8(3) . . ?
C21 C20 C22 110.8(3) . . ?
N3 C20 H20 106.1 . . ?
C21 C20 H20 106.1 . . ?
C22 C20 H20 106.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 C25 115.4(3) . . ?
N3 C23 C24 111.1(3) . . ?
C25 C23 C24 108.4(4) . . ?
N3 C23 H23 107.2 . . ?
C25 C23 H23 107.2 . . ?
C24 C23 H23 107.2 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
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 . . ?
Cl6 C27 Cl5 110.4(3) . . ?
Cl6 C27 H27A 109.6 . . ?
Cl5 C27 H27A 109.6 . . ?
Cl6 C27 H27B 109.6 . . ?
Cl5 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
Cl4 C26 Cl3 112.3(3) . . ?
Cl4 C26 H26A 109.1 . . ?
Cl3 C26 H26A 109.1 . . ?
Cl4 C26 H26B 109.1 . . ?
Cl3 C26 H26B 109.1 . . ?
H26A C26 H26B 107.9 . . ?

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 Pd1 P1 N4 -74.11(15) . . . . ?
Cl1 Pd1 P1 N4 102.26(13) . . . . ?
N2 Pd1 P1 N3 152.44(16) . . . . ?
Cl1 Pd1 P1 N3 -31.19(15) . . . . ?
N2 Pd1 P1 N1 40.47(14) . . . . ?
Cl1 Pd1 P1 N1 -143.16(12) . . . . ?
N4 P1 N1 C1 -83.5(4) . . . . ?
N3 P1 N1 C1 30.3(4) . . . . ?
Pd1 P1 N1 C1 157.7(3) . . . . ?
N4 P1 N1 C4 83.7(3) . . . . ?
N3 P1 N1 C4 -162.4(3) . . . . ?
Pd1 P1 N1 C4 -35.0(3) . . . . ?
P1 Pd1 N2 C5 -36.5(3) . . . . ?
Cl2 Pd1 N2 C5 138.2(3) . . . . ?
P1 Pd1 N2 C6 146.8(2) . . . . ?
Cl2 Pd1 N2 C6 -38.5(3) . . . . ?
N4 P1 N3 C23 -176.4(3) . . . . ?
N1 P1 N3 C23 73.1(3) . . . . ?
Pd1 P1 N3 C23 -42.2(3) . . . . ?
N4 P1 N3 C20 -25.1(3) . . . . ?
N1 P1 N3 C20 -135.6(3) . . . . ?
Pd1 P1 N3 C20 109.1(3) . . . . ?
N3 P1 N4 C14 -62.2(3) . . . . ?
N1 P1 N4 C14 44.0(3) . . . . ?
Pd1 P1 N4 C14 158.6(2) . . . . ?
N3 P1 N4 C17 121.6(3) . . . . ?
N1 P1 N4 C17 -132.3(3) . . . . ?
Pd1 P1 N4 C17 -17.7(3) . . . . ?
C4 N1 C1 C2 0.5(4) . . . . ?
P1 N1 C1 C2 169.7(3) . . . . ?
N1 C1 C2 C3 -0.4(5) . . . . ?
C1 C2 C3 C4 0.1(5) . . . . ?
C2 C3 C4 N1 0.2(5) . . . . ?
C2 C3 C4 C5 -173.7(4) . . . . ?
C1 N1 C4 C3 -0.5(4) . . . . ?
P1 N1 C4 C3 -169.9(3) . . . . ?
C1 N1 C4 C5 173.5(4) . . . . ?
P1 N1 C4 C5 4.0(6) . . . . ?
C6 N2 C5 C4 -171.8(4) . . . . ?
Pd1 N2 C5 C4 11.4(6) . . . . ?
C3 C4 C5 N2 -173.5(4) . . . . ?
N1 C4 C5 N2 13.6(7) . . . . ?
C5 N2 C6 C11 133.6(4) . . . . ?
Pd1 N2 C6 C11 -49.3(4) . . . . ?
C5 N2 C6 C7 -42.9(5) . . . . ?
Pd1 N2 C6 C7 134.2(3) . . . . ?
C11 C6 C7 C8 -1.7(6) . . . . ?
N2 C6 C7 C8 174.8(3) . . . . ?
C6 C7 C8 C9 0.3(6) . . . . ?
C6 C7 C8 C12 -178.8(4) . . . . ?
C7 C8 C9 C10 0.9(6) . . . . ?
C12 C8 C9 C10 -179.9(4) . . . . ?
C8 C9 C10 C11 -0.8(6) . . . . ?
C8 C9 C10 C13 -178.8(4) . . . . ?
C7 C6 C11 C10 1.9(6) . . . . ?
N2 C6 C11 C10 -174.6(3) . . . . ?
C9 C10 C11 C6 -0.6(6) . . . . ?
C13 C10 C11 C6 177.4(4) . . . . ?
C17 N4 C14 C16 -48.1(5) . . . . ?
P1 N4 C14 C16 135.8(3) . . . . ?
C17 N4 C14 C15 80.4(4) . . . . ?
P1 N4 C14 C15 -95.7(4) . . . . ?
C14 N4 C17 C19 79.6(5) . . . . ?
P1 N4 C17 C19 -104.3(4) . . . . ?
C14 N4 C17 C18 -49.5(5) . . . . ?
P1 N4 C17 C18 126.7(3) . . . . ?
C23 N3 C20 C21 37.7(5) . . . . ?
P1 N3 C20 C21 -115.0(4) . . . . ?
C23 N3 C20 C22 -90.1(4) . . . . ?
P1 N3 C20 C22 117.2(3) . . . . ?
C20 N3 C23 C25 -170.6(3) . . . . ?
P1 N3 C23 C25 -18.5(5) . . . . ?
C20 N3 C23 C24 65.6(4) . . . . ?
P1 N3 C23 C24 -142.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.091

#=======================================END

data_16
_database_code_depnum_ccdc_archive 'CCDC 617737'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Bis{(2,4,6-Trimethyl-phenyl)-(pyrrolato)} nickel
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 N4 Ni'
_chemical_formula_sum            'C28 H30 N4 Ni'
_chemical_formula_weight         481.27

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'
Ni Ni 0.3393 1.1124 '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                   10.0308(10)
_cell_length_b                   12.9207(13)
_cell_length_c                   13.9514(14)
_cell_angle_alpha                92.56(1)
_cell_angle_beta                 93.53(1)
_cell_angle_gamma                91.99(1)
_cell_volume                     1801.7(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5655
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      28.98

_exptl_crystal_description       trapetzoid
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             762
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.7867
_exptl_absorpt_correction_T_max  0.9456
_exptl_absorpt_process_details   
'XPREP 6.14 (Bruker,2003), R(int)=0.069 before correction'

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.0400
0.00 -1.00 0.00 0.0400
0.00 1.00 1.00 0.0600
0.00 -1.00 -1.00 0.0600
-1.00 0.00 1.00 0.1400
1.00 0.00 -1.00 0.1400
-1.00 1.00 -1.00 0.1400
1.00 -1.00 1.00 0.1500

_exptl_special_details           
;The data collection nominally covered full sphere of reciprocal
space, by a combination of 4 runs of narrow-frame \w-scans (scan
width 0.3\% \w, 5s exposure), every run at a different \f angle.
Crystal to detector distance 4.44 cm.
;

_diffrn_ambient_temperature      120(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  'Siemens SMART 1K CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_standards_number         0
_diffrn_reflns_number            24988
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         29.00
_reflns_number_total             9511
_reflns_number_gt                7420
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'SMART version 5.054 (Bruker, 1999)'
_computing_cell_refinement       'SAINT version 6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT version 6.45A (Bruker, 2003)'
_computing_structure_solution    'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_refinement  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL version 6.14 (Bruker, 2003)'
_computing_publication_material  'SHELXTL version 6.14 (Bruker, 2003)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. Methyl groups
were refined as rigid bodies rotating around C---C bonds, with a common
refined U for three H atoms. Other H atoms: "riding" model (constr).
;

_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^)+(0.0413P)^2^+0.6282P] 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         9511
_refine_ls_number_parameters     466
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.0943
_refine_ls_wR_factor_gt          0.0881
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Ni1 Ni 0.15350(2) 0.318005(18) 0.116332(16) 0.01528(7) Uani 1 1 d . . .
N1 N -0.03860(15) 0.31293(12) 0.10558(10) 0.0164(3) Uani 1 1 d . . .
N2 N 0.13139(15) 0.42010(11) 0.21642(10) 0.0155(3) Uani 1 1 d . . .
N3 N 0.34380(15) 0.30542(12) 0.13679(11) 0.0175(3) Uani 1 1 d . . .
N4 N 0.17723(15) 0.24387(13) -0.00158(11) 0.0194(3) Uani 1 1 d . . .
C1 C -0.09046(18) 0.38433(14) 0.15951(13) 0.0187(4) Uani 1 1 d . . .
H1 H -0.1843 0.3922 0.1592 0.022 Uiso 1 1 d R . .
C2 C -0.00055(18) 0.44878(15) 0.21790(13) 0.0184(4) Uani 1 1 d . . .
C3 C -0.0095(2) 0.53846(15) 0.27690(14) 0.0228(4) Uani 1 1 d . . .
H3 H -0.0883 0.5738 0.2900 0.027 Uiso 1 1 d R . .
C4 C 0.11996(19) 0.56523(15) 0.31236(14) 0.0214(4) Uani 1 1 d . . .
H4 H 0.1470 0.6229 0.3545 0.026 Uiso 1 1 d R . .
C5 C 0.20310(18) 0.49118(14) 0.27426(13) 0.0177(4) Uani 1 1 d . . .
H5 H 0.2972 0.4909 0.2873 0.021 Uiso 1 1 d R . .
C6 C 0.39749(19) 0.26051(15) 0.06331(13) 0.0213(4) Uani 1 1 d . . .
H6 H 0.4908 0.2500 0.0636 0.026 Uiso 1 1 d R . .
C7 C 0.31024(19) 0.22858(16) -0.01616(13) 0.0207(4) Uani 1 1 d . . .
C8 C 0.3251(2) 0.19061(17) -0.11026(14) 0.0254(4) Uani 1 1 d . . .
H8 H 0.4059 0.1735 -0.1383 0.031 Uiso 1 1 d R . .
C9 C 0.1966(2) 0.18325(16) -0.15401(14) 0.0249(4) Uani 1 1 d . . .
H9 H 0.1726 0.1600 -0.2185 0.030 Uiso 1 1 d R . .
C10 C 0.10926(19) 0.21628(16) -0.08592(13) 0.0225(4) Uani 1 1 d . . .
H10 H 0.0151 0.2190 -0.0973 0.027 Uiso 1 1 d R . .
C11 C -0.12621(17) 0.24170(14) 0.04844(13) 0.0167(4) Uani 1 1 d . . .
C12 C -0.20410(18) 0.27790(15) -0.02924(13) 0.0191(4) Uani 1 1 d . . .
C13 C -0.28494(19) 0.20524(16) -0.08543(14) 0.0228(4) Uani 1 1 d . . .
H13 H -0.3385 0.2283 -0.1383 0.027 Uiso 1 1 d R . .
C14 C -0.28955(19) 0.10064(16) -0.06664(14) 0.0242(4) Uani 1 1 d . . .
C15 C -0.2086(2) 0.06758(16) 0.01005(14) 0.0231(4) Uani 1 1 d . . .
H15 H -0.2100 -0.0040 0.0230 0.028 Uiso 1 1 d R . .
C16 C -0.12608(18) 0.13614(15) 0.06803(13) 0.0194(4) Uani 1 1 d . . .
C17 C -0.1911(2) 0.38848(16) -0.05815(14) 0.0245(4) Uani 1 1 d . . .
H17A H -0.2191 0.4349 -0.0063 0.037(4) Uiso 1 1 d R . .
H17B H -0.2480 0.3973 -0.1167 0.037(4) Uiso 1 1 d R . .
H17C H -0.0978 0.4053 -0.0703 0.037(4) Uiso 1 1 d R . .
C18 C -0.3771(2) 0.02342(18) -0.12832(17) 0.0370(6) Uani 1 1 d . . .
H18A H -0.3307 -0.0417 -0.1358 0.050(5) Uiso 1 1 d R . .
H18B H -0.3966 0.0513 -0.1916 0.050(5) Uiso 1 1 d R . .
H18C H -0.4609 0.0105 -0.0975 0.050(5) Uiso 1 1 d R . .
C19 C -0.0351(2) 0.09736(16) 0.14767(14) 0.0241(4) Uani 1 1 d . . .
H19A H -0.0561 0.0237 0.1557 0.035(4) Uiso 1 1 d R . .
H19B H -0.0481 0.1369 0.2077 0.035(4) Uiso 1 1 d R . .
H19C H 0.0581 0.1063 0.1313 0.035(4) Uiso 1 1 d R . .
C21 C 0.42816(17) 0.34014(14) 0.21910(13) 0.0165(4) Uani 1 1 d . . .
C22 C 0.52257(18) 0.42138(14) 0.21137(13) 0.0176(4) Uani 1 1 d . . .
C23 C 0.59983(18) 0.45623(15) 0.29301(13) 0.0192(4) Uani 1 1 d . . .
H23 H 0.6649 0.5106 0.2882 0.023 Uiso 1 1 d R . .
C24 C 0.58480(18) 0.41376(14) 0.38207(13) 0.0190(4) Uani 1 1 d . . .
C25 C 0.48874(19) 0.33427(14) 0.38753(13) 0.0190(4) Uani 1 1 d . . .
H25 H 0.4767 0.3051 0.4478 0.023 Uiso 1 1 d R . .
C26 C 0.40993(18) 0.29635(14) 0.30754(13) 0.0160(3) Uani 1 1 d . . .
C27 C 0.5357(2) 0.47529(17) 0.11817(14) 0.0267(4) Uani 1 1 d . . .
H27A H 0.5916 0.5388 0.1303 0.039(4) Uiso 1 1 d R . .
H27B H 0.4469 0.4929 0.0919 0.039(4) Uiso 1 1 d R . .
H27C H 0.5771 0.4291 0.0719 0.039(4) Uiso 1 1 d R . .
C28 C 0.6699(2) 0.45454(17) 0.46944(14) 0.0273(4) Uani 1 1 d . . .
H28A H 0.7609 0.4301 0.4656 0.066(5) Uiso 1 1 d R . .
H28B H 0.6318 0.4296 0.5276 0.066(5) Uiso 1 1 d R . .
H28C H 0.6723 0.5305 0.4719 0.066(5) Uiso 1 1 d R . .
C29 C 0.3077(2) 0.20969(15) 0.31677(14) 0.0225(4) Uani 1 1 d . . .
H29A H 0.3109 0.1884 0.3834 0.039(4) Uiso 1 1 d R . .
H29B H 0.3273 0.1506 0.2741 0.039(4) Uiso 1 1 d R . .
H29C H 0.2184 0.2337 0.2988 0.039(4) Uiso 1 1 d R . .
Ni2 Ni 0.5000 0.0000 0.5000 0.01550(8) Uani 1 2 d S . .
N5 N 0.31638(15) -0.00471(12) 0.53619(11) 0.0170(3) Uani 1 1 d . . .
N6 N 0.50858(15) 0.13145(12) 0.56956(11) 0.0172(3) Uani 1 1 d . . .
C31 C 0.28640(19) 0.07965(15) 0.58356(14) 0.0212(4) Uani 1 1 d . . .
H31 H 0.1991 0.0881 0.6049 0.025 Uiso 1 1 d R . .
C32 C 0.38624(19) 0.15711(15) 0.60200(14) 0.0199(4) Uani 1 1 d . . .
C33 C 0.3963(2) 0.25179(15) 0.65502(14) 0.0225(4) Uani 1 1 d . . .
H33 H 0.3265 0.2865 0.6846 0.027 Uiso 1 1 d R . .
C34 C 0.5297(2) 0.28436(15) 0.65538(14) 0.0214(4) Uani 1 1 d . . .
H34 H 0.5692 0.3462 0.6857 0.026 Uiso 1 1 d R . .
C35 C 0.59504(19) 0.20928(14) 0.60290(14) 0.0206(4) Uani 1 1 d . . .
H35 H 0.6876 0.2124 0.5921 0.025 Uiso 1 1 d R . .
C41 C 0.21784(17) -0.08834(14) 0.53193(13) 0.0163(4) Uani 1 1 d . . .
C42 C 0.12669(18) -0.10407(14) 0.45212(13) 0.0186(4) Uani 1 1 d . . .
C43 C 0.03582(18) -0.18799(14) 0.45050(14) 0.0193(4) Uani 1 1 d . . .
H43 H -0.0246 -0.2008 0.3958 0.023 Uiso 1 1 d R . .
C44 C 0.03067(18) -0.25407(14) 0.52676(14) 0.0193(4) Uani 1 1 d . . .
C45 C 0.12163(19) -0.23517(14) 0.60558(13) 0.0202(4) Uani 1 1 d . . .
H45 H 0.1189 -0.2792 0.6582 0.024 Uiso 1 1 d R . .
C46 C 0.21660(18) -0.15356(14) 0.60954(13) 0.0181(4) Uani 1 1 d . . .
C47 C 0.1290(2) -0.03304(16) 0.36903(15) 0.0270(4) Uani 1 1 d . . .
H47A H 0.0727 -0.0638 0.3145 0.049(4) Uiso 1 1 d R . .
H47B H 0.2209 -0.0235 0.3501 0.049(4) Uiso 1 1 d R . .
H47C H 0.0948 0.0343 0.3886 0.049(4) Uiso 1 1 d R . .
C48 C -0.0691(2) -0.34406(16) 0.52301(15) 0.0262(4) Uani 1 1 d . . .
H48A H -0.1554 -0.3225 0.4953 0.051(5) Uiso 1 1 d R . .
H48B H -0.0797 -0.3670 0.5882 0.051(5) Uiso 1 1 d R . .
H48C H -0.0372 -0.4013 0.4831 0.051(5) Uiso 1 1 d R . .
C49 C 0.3133(2) -0.13432(16) 0.69602(14) 0.0244(4) Uani 1 1 d . . .
H49A H 0.2877 -0.0729 0.7333 0.037(4) Uiso 1 1 d R . .
H49B H 0.4037 -0.1230 0.6748 0.037(4) Uiso 1 1 d R . .
H49C H 0.3112 -0.1946 0.7362 0.037(4) Uiso 1 1 d R . .

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
Ni1 0.01302(12) 0.01935(13) 0.01328(11) -0.00153(9) 0.00083(8) 0.00082(9)
N1 0.0148(7) 0.0193(8) 0.0153(7) 0.0009(6) 0.0013(6) 0.0004(6)
N2 0.0152(7) 0.0166(7) 0.0149(7) 0.0003(6) 0.0023(6) -0.0004(6)
N3 0.0159(7) 0.0214(8) 0.0149(7) -0.0011(6) 0.0003(6) 0.0011(6)
N4 0.0163(8) 0.0258(9) 0.0160(7) -0.0023(6) 0.0014(6) 0.0018(6)
C1 0.0166(9) 0.0219(10) 0.0179(9) 0.0008(7) 0.0034(7) 0.0029(7)
C2 0.0158(9) 0.0221(9) 0.0175(9) 0.0010(7) 0.0033(7) 0.0021(7)
C3 0.0209(10) 0.0233(10) 0.0242(10) -0.0042(8) 0.0037(8) 0.0044(8)
C4 0.0240(10) 0.0185(9) 0.0212(9) -0.0029(7) 0.0020(8) -0.0015(8)
C5 0.0173(9) 0.0183(9) 0.0175(9) 0.0023(7) 0.0009(7) -0.0017(7)
C6 0.0160(9) 0.0293(11) 0.0189(9) 0.0000(8) 0.0020(7) 0.0034(8)
C7 0.0163(9) 0.0277(10) 0.0179(9) -0.0022(8) 0.0023(7) 0.0007(8)
C8 0.0214(10) 0.0355(12) 0.0193(9) -0.0046(8) 0.0049(8) 0.0017(9)
C9 0.0238(10) 0.0340(12) 0.0162(9) -0.0047(8) 0.0013(8) -0.0013(8)
C10 0.0187(9) 0.0316(11) 0.0166(9) -0.0023(8) -0.0003(7) 0.0007(8)
C11 0.0128(8) 0.0219(9) 0.0154(8) -0.0015(7) 0.0029(7) 0.0001(7)
C12 0.0158(9) 0.0242(10) 0.0178(9) 0.0004(7) 0.0035(7) 0.0033(7)
C13 0.0181(9) 0.0324(11) 0.0175(9) -0.0014(8) -0.0024(7) 0.0048(8)
C14 0.0192(9) 0.0288(11) 0.0236(10) -0.0079(8) -0.0008(8) 0.0003(8)
C15 0.0238(10) 0.0207(10) 0.0244(10) -0.0016(8) 0.0011(8) 0.0002(8)
C16 0.0168(9) 0.0230(10) 0.0186(9) -0.0005(7) 0.0029(7) 0.0024(7)
C17 0.0246(10) 0.0268(11) 0.0225(10) 0.0060(8) 0.0008(8) 0.0024(8)
C18 0.0330(12) 0.0357(13) 0.0392(13) -0.0141(10) -0.0124(10) 0.0023(10)
C19 0.0262(10) 0.0216(10) 0.0242(10) 0.0025(8) -0.0033(8) 0.0024(8)
C21 0.0139(8) 0.0203(9) 0.0151(8) -0.0012(7) -0.0008(6) 0.0032(7)
C22 0.0137(8) 0.0210(9) 0.0187(9) 0.0024(7) 0.0027(7) 0.0032(7)
C23 0.0141(8) 0.0192(9) 0.0244(9) 0.0018(7) 0.0015(7) -0.0005(7)
C24 0.0176(9) 0.0190(9) 0.0198(9) -0.0024(7) -0.0018(7) 0.0016(7)
C25 0.0226(9) 0.0181(9) 0.0161(8) 0.0005(7) 0.0000(7) 0.0016(7)
C26 0.0158(8) 0.0154(8) 0.0167(8) -0.0006(7) 0.0014(7) 0.0018(7)
C27 0.0212(10) 0.0362(12) 0.0234(10) 0.0109(9) 0.0023(8) -0.0013(9)
C28 0.0279(11) 0.0291(11) 0.0233(10) -0.0032(8) -0.0043(8) -0.0049(9)
C29 0.0259(10) 0.0203(10) 0.0208(9) 0.0011(7) 0.0002(8) -0.0044(8)
Ni2 0.01364(16) 0.01363(16) 0.01919(17) -0.00097(12) 0.00276(12) -0.00097(12)
N5 0.0142(7) 0.0148(7) 0.0221(8) -0.0004(6) 0.0033(6) -0.0011(6)
N6 0.0164(7) 0.0153(7) 0.0200(8) -0.0002(6) 0.0035(6) 0.0003(6)
C31 0.0172(9) 0.0184(9) 0.0282(10) -0.0027(8) 0.0064(8) 0.0003(7)
C32 0.0181(9) 0.0179(9) 0.0241(9) -0.0008(7) 0.0065(7) 0.0002(7)
C33 0.0239(10) 0.0181(9) 0.0261(10) -0.0025(8) 0.0095(8) 0.0003(8)
C34 0.0265(10) 0.0163(9) 0.0209(9) -0.0020(7) 0.0023(8) -0.0025(8)
C35 0.0178(9) 0.0187(9) 0.0250(10) -0.0004(8) 0.0025(7) -0.0018(7)
C41 0.0132(8) 0.0136(8) 0.0224(9) -0.0018(7) 0.0046(7) -0.0002(7)
C42 0.0152(9) 0.0184(9) 0.0227(9) 0.0019(7) 0.0034(7) 0.0018(7)
C43 0.0150(9) 0.0195(9) 0.0230(9) -0.0017(7) 0.0003(7) 0.0007(7)
C44 0.0183(9) 0.0151(9) 0.0247(9) -0.0032(7) 0.0072(7) -0.0009(7)
C45 0.0241(10) 0.0182(9) 0.0191(9) 0.0021(7) 0.0060(7) 0.0006(7)
C46 0.0187(9) 0.0163(9) 0.0195(9) -0.0009(7) 0.0032(7) 0.0021(7)
C47 0.0257(11) 0.0250(11) 0.0300(11) 0.0082(9) -0.0036(8) -0.0046(8)
C48 0.0274(11) 0.0215(10) 0.0294(11) -0.0018(8) 0.0061(8) -0.0083(8)
C49 0.0245(10) 0.0239(10) 0.0244(10) -0.0001(8) -0.0010(8) 0.0007(8)

_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
Ni1 N4 1.8983(15) . ?
Ni1 N2 1.9061(15) . ?
Ni1 N1 1.9221(15) . ?
Ni1 N3 1.9262(15) . ?
N1 C1 1.307(2) . ?
N1 C11 1.431(2) . ?
N2 C5 1.352(2) . ?
N2 C2 1.388(2) . ?
N3 C6 1.309(2) . ?
N3 C21 1.430(2) . ?
N4 C10 1.350(2) . ?
N4 C7 1.382(2) . ?
C1 C2 1.403(3) . ?
C2 C3 1.400(3) . ?
C3 C4 1.387(3) . ?
C4 C5 1.399(3) . ?
C6 C7 1.407(3) . ?
C7 C8 1.399(3) . ?
C8 C9 1.390(3) . ?
C9 C10 1.394(3) . ?
C11 C16 1.403(3) . ?
C11 C12 1.404(3) . ?
C12 C13 1.399(3) . ?
C12 C17 1.505(3) . ?
C13 C14 1.388(3) . ?
C14 C15 1.394(3) . ?
C14 C18 1.509(3) . ?
C15 C16 1.388(3) . ?
C16 C19 1.509(3) . ?
C21 C26 1.399(2) . ?
C21 C22 1.401(3) . ?
C22 C23 1.386(3) . ?
C22 C27 1.513(3) . ?
C23 C24 1.395(3) . ?
C24 C25 1.391(3) . ?
C24 C28 1.509(3) . ?
C25 C26 1.388(2) . ?
C26 C29 1.507(3) . ?
Ni2 N6 1.9148(15) . ?
Ni2 N6 1.9149(15) 2_656 ?
Ni2 N5 1.9392(15) . ?
Ni2 N5 1.9393(15) 2_656 ?
N5 C31 1.303(2) . ?
N5 C41 1.436(2) . ?
N6 C35 1.352(2) . ?
N6 C32 1.380(2) . ?
C31 C32 1.395(3) . ?
C32 C33 1.398(3) . ?
C33 C34 1.388(3) . ?
C34 C35 1.395(3) . ?
C41 C42 1.400(3) . ?
C41 C46 1.402(3) . ?
C42 C43 1.391(3) . ?
C42 C47 1.511(3) . ?
C43 C44 1.396(3) . ?
C44 C45 1.392(3) . ?
C44 C48 1.505(3) . ?
C45 C46 1.393(3) . ?
C46 C49 1.507(3) . ?

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
N4 Ni1 N2 166.48(7) . . ?
N4 Ni1 N1 96.56(6) . . ?
N2 Ni1 N1 83.80(6) . . ?
N4 Ni1 N3 83.80(7) . . ?
N2 Ni1 N3 97.74(6) . . ?
N1 Ni1 N3 171.92(7) . . ?
C1 N1 C11 118.83(15) . . ?
C1 N1 Ni1 113.03(13) . . ?
C11 N1 Ni1 128.14(12) . . ?
C5 N2 C2 105.81(15) . . ?
C5 N2 Ni1 140.80(13) . . ?
C2 N2 Ni1 111.38(12) . . ?
C6 N3 C21 119.00(16) . . ?
C6 N3 Ni1 112.92(12) . . ?
C21 N3 Ni1 128.07(12) . . ?
C10 N4 C7 105.98(15) . . ?
C10 N4 Ni1 140.11(14) . . ?
C7 N4 Ni1 112.47(12) . . ?
N1 C1 C2 116.61(17) . . ?
N2 C2 C3 110.23(16) . . ?
N2 C2 C1 113.96(16) . . ?
C3 C2 C1 135.78(18) . . ?
C4 C3 C2 106.12(17) . . ?
C3 C4 C5 107.03(17) . . ?
N2 C5 C4 110.80(16) . . ?
N3 C6 C7 116.73(17) . . ?
N4 C7 C8 110.59(16) . . ?
N4 C7 C6 113.69(16) . . ?
C8 C7 C6 135.56(18) . . ?
C9 C8 C7 105.42(17) . . ?
C8 C9 C10 107.50(17) . . ?
N4 C10 C9 110.51(17) . . ?
C16 C11 C12 121.56(17) . . ?
C16 C11 N1 118.97(16) . . ?
C12 C11 N1 119.36(16) . . ?
C13 C12 C11 117.64(18) . . ?
C13 C12 C17 120.44(17) . . ?
C11 C12 C17 121.60(17) . . ?
C14 C13 C12 122.25(18) . . ?
C13 C14 C15 118.28(18) . . ?
C13 C14 C18 121.44(19) . . ?
C15 C14 C18 120.26(19) . . ?
C16 C15 C14 121.96(19) . . ?
C15 C16 C11 118.27(17) . . ?
C15 C16 C19 120.70(18) . . ?
C11 C16 C19 120.99(17) . . ?
C26 C21 C22 120.95(16) . . ?
C26 C21 N3 119.35(16) . . ?
C22 C21 N3 119.60(16) . . ?
C23 C22 C21 118.54(17) . . ?
C23 C22 C27 119.81(17) . . ?
C21 C22 C27 121.56(17) . . ?
C22 C23 C24 121.93(17) . . ?
C25 C24 C23 118.05(17) . . ?
C25 C24 C28 121.62(17) . . ?
C23 C24 C28 120.32(17) . . ?
C26 C25 C24 122.00(17) . . ?
C25 C26 C21 118.52(17) . . ?
C25 C26 C29 120.14(16) . . ?
C21 C26 C29 121.33(16) . . ?
N6 Ni2 N6 179.999(1) . 2_656 ?
N6 Ni2 N5 83.68(6) . . ?
N6 Ni2 N5 96.32(6) 2_656 . ?
N6 Ni2 N5 96.32(6) . 2_656 ?
N6 Ni2 N5 83.68(6) 2_656 2_656 ?
N5 Ni2 N5 180.0 . 2_656 ?
C31 N5 C41 115.99(15) . . ?
C31 N5 Ni2 112.12(12) . . ?
C41 N5 Ni2 131.19(12) . . ?
C35 N6 C32 105.66(15) . . ?
C35 N6 Ni2 142.25(13) . . ?
C32 N6 Ni2 112.01(12) . . ?
N5 C31 C32 118.03(17) . . ?
N6 C32 C31 113.97(16) . . ?
N6 C32 C33 110.79(16) . . ?
C31 C32 C33 134.83(18) . . ?
C34 C33 C32 105.54(17) . . ?
C33 C34 C35 107.26(17) . . ?
N6 C35 C34 110.74(17) . . ?
C42 C41 C46 121.39(16) . . ?
C42 C41 N5 120.61(16) . . ?
C46 C41 N5 118.00(16) . . ?
C43 C42 C41 118.22(17) . . ?
C43 C42 C47 120.93(17) . . ?
C41 C42 C47 120.83(17) . . ?
C42 C43 C44 122.05(17) . . ?
C45 C44 C43 118.12(17) . . ?
C45 C44 C48 121.07(18) . . ?
C43 C44 C48 120.81(17) . . ?
C44 C45 C46 121.94(18) . . ?
C45 C46 C41 118.26(17) . . ?
C45 C46 C49 120.88(17) . . ?
C41 C46 C49 120.85(17) . . ?

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 C2 C1 N1 -6.0(2) . . . . ?
C2 C1 N1 C11 176.79(16) . . . . ?
C1 N1 C11 C12 68.2(2) . . . . ?
N4 C7 C6 N3 -4.0(3) . . . . ?
C7 C6 N3 C21 -179.48(17) . . . . ?
C6 N3 C21 C22 66.4(2) . . . . ?
N6 C32 C31 N5 -2.3(3) . . . . ?
C32 C31 N5 C41 170.61(17) . . . . ?
C31 N5 C41 C42 96.8(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.066

#=====================================END