data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Mir Wais Hosseini'
'Stephane Baudron'
'Catherine Bronner'
'Luisa De Cola'
'Aurelie Guenet'
'Cristian Strassert'

_publ_contact_author_name        'Mir Wais Hosseini'
_publ_contact_author_email       HOSSEINI@CHIMIE.U-STRASBG.FR

_publ_section_title              
;
Dipyrrin based luminescent cyclometallated palladium
and platinum complexes
;

# Attachment 'Hosseini_Baudron.cif'

##########################Paper No. X/XXXXXX##############################

data_compound5
_database_code_depnum_ccdc_archive 'CCDC 729823'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H25 N3 Pt'
_chemical_formula_sum            'C29 H25 N3 Pt'
_chemical_formula_weight         610.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7030 8.3910 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P2(1)2(1)2(1) '
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   7.8866(3)
_cell_length_b                   14.9148(6)
_cell_length_c                   19.3528(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2276.41(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2358
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      26.66

_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    6.187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3566
_exptl_absorpt_correction_T_max  0.6713
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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            11628
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4811
_reflns_number_gt                4305
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0051P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(11)
_refine_ls_number_reflns         4811
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0669
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_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
C1 C 0.7397(9) 0.1683(5) 0.0761(4) 0.023(2) Uani 1 1 d . . .
H1 H 0.8352 0.1467 0.0533 0.027 Uiso 1 1 calc R . .
C2 C 0.6549(11) 0.2405(5) 0.0479(4) 0.029(2) Uani 1 1 d . . .
H2 H 0.6935 0.2666 0.0072 0.035 Uiso 1 1 calc R . .
C3 C 0.5121(11) 0.2739(5) 0.0805(4) 0.030(2) Uani 1 1 d . . .
H3 H 0.4562 0.3237 0.0627 0.036 Uiso 1 1 calc R . .
C4 C 0.4536(11) 0.2333(5) 0.1392(4) 0.026(2) Uani 1 1 d . . .
H4 H 0.3565 0.2551 0.1607 0.032 Uiso 1 1 calc R . .
C5 C 0.5384(10) 0.1588(5) 0.1675(4) 0.0189(18) Uani 1 1 d . . .
C6 C 0.4707(9) 0.1042(5) 0.2240(4) 0.0194(18) Uani 1 1 d . . .
C7 C 0.3139(11) 0.1144(5) 0.2547(4) 0.0226(18) Uani 1 1 d . . .
H7 H 0.2461 0.1632 0.2432 0.027 Uiso 1 1 calc R . .
C8 C 0.2573(8) 0.0525(5) 0.3027(4) 0.027(2) Uani 1 1 d . . .
H8 H 0.1523 0.0599 0.3238 0.032 Uiso 1 1 calc R . .
C9 C 0.3564(8) -0.0198(5) 0.3188(4) 0.0256(19) Uani 1 1 d . . .
H9 H 0.3178 -0.0633 0.3495 0.031 Uiso 1 1 calc R . .
C10 C 0.5160(9) -0.0274(5) 0.2887(3) 0.0213(17) Uani 1 1 d . . .
H10 H 0.5841 -0.0760 0.3004 0.026 Uiso 1 1 calc R . .
N1 N 0.5758(7) 0.0341(5) 0.2427(3) 0.0203(14) Uani 1 1 d . . .
C12 C 1.1059(10) 0.0801(5) 0.1010(4) 0.0238(19) Uani 1 1 d . . .
H12 H 1.0887 0.1416 0.1043 0.029 Uiso 1 1 calc R . .
C13 C 1.2263(10) 0.0401(5) 0.0576(3) 0.0238(19) Uani 1 1 d . . .
H13 H 1.3018 0.0693 0.0284 0.029 Uiso 1 1 calc R . .
C14 C 1.2104(11) -0.0514(4) 0.0671(4) 0.0238(19) Uani 1 1 d . . .
H14 H 1.2715 -0.0957 0.0442 0.029 Uiso 1 1 calc R . .
C15 C 1.0825(10) -0.0654(5) 0.1184(4) 0.0172(18) Uani 1 1 d . . .
C16 C 1.0635(9) -0.1438(5) 0.1577(4) 0.0151(17) Uani 1 1 d . . .
C17 C 0.9924(9) -0.1453(5) 0.2237(4) 0.0168(17) Uani 1 1 d . . .
C18 C 1.0285(9) -0.2071(5) 0.2777(4) 0.0150(17) Uani 1 1 d . . .
H18 H 1.0793 -0.2630 0.2729 0.018 Uiso 1 1 calc R . .
C19 C 0.9745(10) -0.1690(5) 0.3380(4) 0.0235(19) Uani 1 1 d . . .
H19 H 0.9855 -0.1929 0.3822 0.028 Uiso 1 1 calc R . .
C20 C 0.8993(9) -0.0870(5) 0.3205(4) 0.0205(17) Uani 1 1 d . . .
H20 H 0.8483 -0.0483 0.3519 0.025 Uiso 1 1 calc R . .
C21 C 1.1314(10) -0.2301(5) 0.1272(4) 0.0172(18) Uani 1 1 d . . .
C22 C 1.3029(11) -0.2548(4) 0.1358(4) 0.0193(17) Uani 1 1 d . . .
C23 C 1.3589(10) -0.3344(5) 0.1054(4) 0.024(2) Uani 1 1 d . . .
H23 H 1.4720 -0.3509 0.1103 0.029 Uiso 1 1 calc R . .
C24 C 1.2516(9) -0.3893(4) 0.0682(4) 0.0178(19) Uani 1 1 d . . .
C25 C 1.0839(10) -0.3642(5) 0.0621(4) 0.0212(19) Uani 1 1 d . . .
H25 H 1.0104 -0.4017 0.0381 0.025 Uiso 1 1 calc R . .
C26 C 1.0198(10) -0.2852(5) 0.0903(4) 0.0200(18) Uani 1 1 d . . .
C27 C 1.4236(10) -0.1951(5) 0.1771(5) 0.032(2) Uani 1 1 d . . .
H27A H 1.3720 -0.1795 0.2204 0.048 Uiso 1 1 calc R . .
H27B H 1.4472 -0.1415 0.1514 0.048 Uiso 1 1 calc R . .
H27C H 1.5275 -0.2269 0.1855 0.048 Uiso 1 1 calc R . .
C28 C 1.3152(10) -0.4726(5) 0.0318(3) 0.0280(17) Uani 1 1 d . . .
H28A H 1.3473 -0.4577 -0.0146 0.042 Uiso 1 1 calc R . .
H28B H 1.2269 -0.5169 0.0309 0.042 Uiso 1 1 calc R . .
H28C H 1.4116 -0.4960 0.0561 0.042 Uiso 1 1 calc R . .
C29 C 0.8353(10) -0.2591(5) 0.0802(4) 0.027(2) Uani 1 1 d . . .
H29A H 0.8291 -0.2053 0.0531 0.041 Uiso 1 1 calc R . .
H29B H 0.7835 -0.2490 0.1244 0.041 Uiso 1 1 calc R . .
H29C H 0.7766 -0.3065 0.0566 0.041 Uiso 1 1 calc R . .
C11 C 0.6896(10) 0.1262(4) 0.1369(3) 0.0124(15) Uani 1 1 d . . .
N2 N 1.0189(7) 0.0194(4) 0.1371(3) 0.0187(14) Uani 1 1 d . . .
N3 N 0.9105(7) -0.0719(4) 0.2533(3) 0.0167(14) Uani 1 1 d . . .
Pt1 Pt 0.80094(4) 0.028161(17) 0.192248(15) 0.01534(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
C1 0.026(6) 0.025(4) 0.018(4) -0.009(3) -0.008(4) 0.003(3)
C2 0.037(7) 0.021(4) 0.029(5) 0.004(4) -0.011(4) -0.004(4)
C3 0.034(6) 0.026(5) 0.029(5) -0.004(4) -0.021(5) 0.009(4)
C4 0.027(5) 0.017(4) 0.035(6) -0.002(4) -0.003(4) 0.007(4)
C5 0.019(5) 0.021(4) 0.017(4) -0.006(3) -0.003(3) 0.002(3)
C6 0.007(4) 0.024(4) 0.027(5) -0.007(3) -0.002(4) -0.004(3)
C7 0.018(4) 0.030(4) 0.020(4) -0.009(3) -0.002(4) 0.003(4)
C8 0.010(4) 0.040(5) 0.031(5) -0.014(4) 0.010(4) 0.001(3)
C9 0.024(5) 0.029(4) 0.024(5) -0.004(4) 0.005(4) -0.003(4)
C10 0.025(4) 0.016(3) 0.022(4) -0.004(4) -0.002(3) -0.005(4)
N1 0.018(3) 0.023(3) 0.020(3) -0.005(3) -0.002(3) 0.002(3)
C12 0.025(5) 0.014(4) 0.033(5) 0.006(3) 0.000(4) 0.003(4)
C13 0.022(5) 0.028(4) 0.021(4) 0.005(3) 0.005(4) -0.002(4)
C14 0.023(4) 0.026(4) 0.021(4) 0.001(3) 0.008(4) 0.006(4)
C15 0.016(4) 0.024(4) 0.012(4) -0.004(3) 0.003(4) 0.000(3)
C16 0.009(4) 0.017(4) 0.020(4) 0.003(3) -0.007(3) 0.002(3)
C17 0.010(4) 0.017(4) 0.023(5) 0.004(3) 0.001(4) 0.001(3)
C18 0.009(4) 0.020(4) 0.016(4) 0.004(3) 0.000(3) 0.002(3)
C19 0.017(5) 0.029(5) 0.025(5) 0.002(4) 0.009(4) 0.002(4)
C20 0.018(4) 0.026(4) 0.018(5) -0.006(3) 0.003(4) 0.001(3)
C21 0.027(5) 0.018(4) 0.007(4) -0.002(3) 0.004(3) 0.003(3)
C22 0.012(4) 0.019(4) 0.027(5) 0.001(3) -0.001(4) -0.001(4)
C23 0.019(5) 0.021(4) 0.033(5) 0.000(4) 0.004(4) 0.008(3)
C24 0.026(5) 0.014(3) 0.013(4) 0.005(3) 0.005(3) 0.006(3)
C25 0.027(5) 0.014(4) 0.023(5) 0.003(3) -0.004(4) -0.006(3)
C26 0.018(5) 0.020(4) 0.022(5) 0.005(3) -0.002(4) -0.003(3)
C27 0.023(5) 0.026(5) 0.048(7) -0.012(4) -0.008(5) 0.000(4)
C28 0.038(5) 0.025(4) 0.021(4) -0.008(4) 0.009(4) 0.010(5)
C29 0.018(5) 0.027(4) 0.036(5) 0.000(4) -0.002(4) 0.002(3)
C11 0.014(4) 0.015(3) 0.008(3) -0.004(3) -0.004(4) -0.005(3)
N2 0.024(4) 0.014(3) 0.018(3) 0.000(3) -0.003(3) 0.004(3)
N3 0.011(3) 0.019(3) 0.020(4) -0.002(3) 0.006(3) 0.000(3)
Pt1 0.01626(14) 0.01364(11) 0.01611(13) -0.00089(13) 0.00044(15) 0.00267(13)

_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
C1 C2 1.381(10) . ?
C1 C11 1.390(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.384(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.368(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.408(10) . ?
C4 H4 0.9300 . ?
C5 C11 1.418(10) . ?
C5 C6 1.463(10) . ?
C6 C7 1.381(10) . ?
C6 N1 1.383(9) . ?
C7 C8 1.383(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.368(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.391(9) . ?
C9 H9 0.9300 . ?
C10 N1 1.362(9) . ?
C10 H10 0.9300 . ?
N1 Pt1 2.029(6) . ?
C12 N2 1.333(9) . ?
C12 C13 1.401(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.432(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.402(10) . ?
C15 N2 1.408(9) . ?
C16 C17 1.396(9) . ?
C16 C21 1.515(9) . ?
C17 N3 1.393(9) . ?
C17 C18 1.422(9) . ?
C18 C19 1.365(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.402(10) . ?
C19 H19 0.9300 . ?
C20 N3 1.322(9) . ?
C20 H20 0.9300 . ?
C21 C26 1.400(10) . ?
C21 C22 1.412(11) . ?
C22 C23 1.397(9) . ?
C22 C27 1.528(10) . ?
C23 C24 1.380(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.379(10) . ?
C24 C28 1.514(9) . ?
C25 C26 1.393(10) . ?
C25 H25 0.9300 . ?
C26 C29 1.519(11) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C11 Pt1 2.014(7) . ?
N2 Pt1 2.027(6) . ?
N3 Pt1 2.091(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C11 123.3(8) . . ?
C2 C1 H1 118.4 . . ?
C11 C1 H1 118.4 . . ?
C1 C2 C3 119.7(8) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 119.6(8) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.8(8) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C11 120.5(7) . . ?
C4 C5 C6 123.8(7) . . ?
C11 C5 C6 115.4(7) . . ?
C7 C6 N1 120.5(7) . . ?
C7 C6 C5 126.0(7) . . ?
N1 C6 C5 113.4(7) . . ?
C6 C7 C8 120.3(7) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 119.7(7) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 119.0(8) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N1 C10 C9 122.2(7) . . ?
N1 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 N1 C6 118.2(6) . . ?
C10 N1 Pt1 126.0(5) . . ?
C6 N1 Pt1 115.6(5) . . ?
N2 C12 C13 112.0(7) . . ?
N2 C12 H12 124.0 . . ?
C13 C12 H12 124.0 . . ?
C14 C13 C12 106.2(7) . . ?
C14 C13 H13 126.9 . . ?
C12 C13 H13 126.9 . . ?
C13 C14 C15 107.4(7) . . ?
C13 C14 H14 126.3 . . ?
C15 C14 H14 126.3 . . ?
C16 C15 N2 124.9(7) . . ?
C16 C15 C14 125.0(7) . . ?
N2 C15 C14 107.3(6) . . ?
C17 C16 C15 123.5(7) . . ?
C17 C16 C21 119.1(6) . . ?
C15 C16 C21 117.4(7) . . ?
N3 C17 C16 123.4(7) . . ?
N3 C17 C18 107.4(6) . . ?
C16 C17 C18 127.1(7) . . ?
C19 C18 C17 107.3(7) . . ?
C19 C18 H18 126.4 . . ?
C17 C18 H18 126.4 . . ?
C18 C19 C20 106.7(7) . . ?
C18 C19 H19 126.6 . . ?
C20 C19 H19 126.6 . . ?
N3 C20 C19 111.0(7) . . ?
N3 C20 H20 124.5 . . ?
C19 C20 H20 124.5 . . ?
C26 C21 C22 120.7(7) . . ?
C26 C21 C16 118.4(7) . . ?
C22 C21 C16 120.9(7) . . ?
C23 C22 C21 118.3(7) . . ?
C23 C22 C27 121.2(8) . . ?
C21 C22 C27 120.5(7) . . ?
C24 C23 C22 122.0(7) . . ?
C24 C23 H23 119.0 . . ?
C22 C23 H23 119.0 . . ?
C25 C24 C23 118.1(7) . . ?
C25 C24 C28 120.0(7) . . ?
C23 C24 C28 121.8(7) . . ?
C24 C25 C26 123.0(7) . . ?
C24 C25 H25 118.5 . . ?
C26 C25 H25 118.5 . . ?
C25 C26 C21 117.9(7) . . ?
C25 C26 C29 121.0(7) . . ?
C21 C26 C29 121.2(7) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C1 C11 C5 116.0(7) . . ?
C1 C11 Pt1 130.8(6) . . ?
C5 C11 Pt1 113.1(5) . . ?
C12 N2 C15 107.0(6) . . ?
C12 N2 Pt1 132.0(5) . . ?
C15 N2 Pt1 119.7(5) . . ?
C20 N3 C17 107.6(6) . . ?
C20 N3 Pt1 130.5(5) . . ?
C17 N3 Pt1 121.3(5) . . ?
C11 Pt1 N2 97.8(3) . . ?
C11 Pt1 N1 80.9(3) . . ?
N2 Pt1 N1 176.8(2) . . ?
C11 Pt1 N3 177.6(3) . . ?
N2 Pt1 N3 84.3(2) . . ?
N1 Pt1 N3 97.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.944
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.180

#===END

###Material relevant to compound 6 at 173K ##

data_compound6
_database_code_depnum_ccdc_archive 'CCDC 729824'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H18 N4 Pt'
_chemical_formula_sum            'C27 H18 N4 Pt'
_chemical_formula_weight         593.54

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'
Pt Pt -1.7033 8.3905 '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 '
_symmetry_space_group_name_Hall  '-P 2yn'
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                   7.2660(3)
_cell_length_b                   12.5451(4)
_cell_length_c                   22.3968(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.177(2)
_cell_angle_gamma                90.00
_cell_volume                     2041.52(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5501
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      26.76

_exptl_crystal_description       platelet
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    6.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3541
_exptl_absorpt_correction_T_max  0.6084
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            18358
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4688
_reflns_number_gt                3898
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4688
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0670
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.1449(7) -0.1394(4) 0.1561(2) 0.0210(12) Uani 1 1 d . . .
H1 H 1.0914 -0.1594 0.1920 0.025 Uiso 1 1 calc R . .
C2 C 1.2960(7) -0.1939(5) 0.1365(3) 0.0260(13) Uani 1 1 d . . .
H2 H 1.3448 -0.2493 0.1591 0.031 Uiso 1 1 calc R . .
C3 C 1.3765(7) -0.1660(5) 0.0822(3) 0.0267(13) Uani 1 1 d . . .
H3 H 1.4750 -0.2049 0.0672 0.032 Uiso 1 1 calc R . .
C4 C 1.3074(7) -0.0792(5) 0.0510(3) 0.0253(13) Uani 1 1 d . . .
H4 H 1.3610 -0.0589 0.0151 0.030 Uiso 1 1 calc R . .
C5 C 1.1572(7) -0.0223(4) 0.0735(3) 0.0177(11) Uani 1 1 d . . .
C6 C 1.0942(7) 0.0795(4) 0.0508(2) 0.0179(11) Uani 1 1 d . . .
C7 C 1.1753(7) 0.1341(5) 0.0038(2) 0.0212(12) Uani 1 1 d . . .
H7 H 1.2636 0.1007 -0.0196 0.025 Uiso 1 1 calc R . .
C8 C 1.1244(7) 0.2389(5) -0.0084(3) 0.0268(13) Uani 1 1 d . . .
H8 H 1.1760 0.2754 -0.0404 0.032 Uiso 1 1 calc R . .
C9 C 0.9967(7) 0.2877(5) 0.0276(3) 0.0261(13) Uani 1 1 d . . .
H9 H 0.9665 0.3589 0.0216 0.031 Uiso 1 1 calc R . .
C10 C 0.9130(7) 0.2304(5) 0.0729(2) 0.0222(12) Uani 1 1 d . . .
H10 H 0.8275 0.2645 0.0971 0.027 Uiso 1 1 calc R . .
C11 C 0.9521(6) 0.1250(4) 0.0833(2) 0.0115(10) Uani 1 1 d . . .
C12 C 0.7503(7) -0.1926(4) 0.2005(3) 0.0228(12) Uani 1 1 d . . .
H12 H 0.8263 -0.2300 0.1745 0.027 Uiso 1 1 calc R . .
C13 C 0.6606(7) -0.2386(5) 0.2495(3) 0.0255(13) Uani 1 1 d . . .
H13 H 0.6675 -0.3094 0.2617 0.031 Uiso 1 1 calc R . .
C14 C 0.5616(7) -0.1594(4) 0.2759(2) 0.0219(12) Uani 1 1 d . . .
H14 H 0.4888 -0.1654 0.3098 0.026 Uiso 1 1 calc R . .
C15 C 0.5909(6) -0.0656(4) 0.2414(2) 0.0172(11) Uani 1 1 d . . .
C16 C 0.4832(7) 0.0281(4) 0.2438(2) 0.0162(11) Uani 1 1 d . . .
C17 C 0.4790(6) 0.1074(4) 0.1999(2) 0.0165(11) Uani 1 1 d . . .
C18 C 0.3492(7) 0.1915(4) 0.1935(3) 0.0220(12) Uani 1 1 d . . .
H18 H 0.2646 0.2134 0.2221 0.026 Uiso 1 1 calc R . .
C19 C 0.3712(7) 0.2341(5) 0.1380(3) 0.0232(13) Uani 1 1 d . . .
H19 H 0.3027 0.2888 0.1208 0.028 Uiso 1 1 calc R . .
C20 C 0.5186(7) 0.1786(4) 0.1120(2) 0.0203(12) Uani 1 1 d . . .
H20 H 0.5629 0.1921 0.0739 0.024 Uiso 1 1 calc R . .
C21 C 0.3410(7) 0.0321(4) 0.2919(2) 0.0178(12) Uani 1 1 d . . .
C22 C 0.3882(7) 0.0334(4) 0.3529(3) 0.0218(13) Uani 1 1 d . . .
H22 H 0.5112 0.0372 0.3643 0.026 Uiso 1 1 calc R . .
C23 C 0.2532(8) 0.0291(4) 0.3961(3) 0.0235(13) Uani 1 1 d . . .
H23 H 0.2852 0.0308 0.4363 0.028 Uiso 1 1 calc R . .
C24 C 0.0692(8) 0.0222(4) 0.3792(3) 0.0199(12) Uani 1 1 d . . .
C25 C 0.0193(7) 0.0216(4) 0.3189(3) 0.0225(13) Uani 1 1 d . . .
H25 H -0.1038 0.0167 0.3078 0.027 Uiso 1 1 calc R . .
C26 C 0.1548(7) 0.0283(4) 0.2763(3) 0.0197(12) Uani 1 1 d . . .
H26 H 0.1216 0.0303 0.2362 0.024 Uiso 1 1 calc R . .
C27 C -0.0777(8) 0.0154(5) 0.4227(3) 0.0263(13) Uani 1 1 d . . .
N1 N 1.0688(6) -0.0559(4) 0.1245(2) 0.0220(10) Uani 1 1 d . . .
N2 N 0.7132(5) -0.0883(3) 0.19549(19) 0.0164(9) Uani 1 1 d . . .
N3 N 0.5876(5) 0.1044(3) 0.14813(19) 0.0164(9) Uani 1 1 d . . .
N4 N -0.1998(8) 0.0105(5) 0.4538(3) 0.0417(15) Uani 1 1 d . . .
Pt1 Pt 0.82897(2) 0.021791(16) 0.139693(9) 0.01454(8) 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
C1 0.021(3) 0.020(3) 0.022(3) -0.001(2) 0.001(2) -0.003(2)
C2 0.022(3) 0.020(3) 0.037(4) -0.002(3) -0.005(3) 0.001(2)
C3 0.021(3) 0.024(3) 0.036(4) -0.001(3) 0.006(2) 0.001(2)
C4 0.024(3) 0.025(3) 0.027(3) -0.003(3) 0.012(2) -0.005(2)
C5 0.017(2) 0.019(3) 0.017(3) -0.001(2) 0.001(2) -0.005(2)
C6 0.021(2) 0.017(3) 0.016(3) -0.001(2) 0.001(2) -0.003(2)
C7 0.021(3) 0.028(3) 0.015(3) -0.001(2) 0.005(2) -0.003(2)
C8 0.027(3) 0.029(3) 0.025(3) 0.007(3) 0.002(2) -0.003(2)
C9 0.028(3) 0.023(3) 0.027(3) 0.005(3) -0.003(2) -0.003(2)
C10 0.017(2) 0.032(3) 0.017(3) -0.005(2) -0.002(2) -0.003(2)
C11 0.016(2) 0.009(2) 0.010(2) 0.0005(19) 0.0002(18) -0.0026(18)
C12 0.019(2) 0.018(3) 0.032(3) 0.001(3) 0.002(2) 0.000(2)
C13 0.019(3) 0.021(3) 0.036(4) 0.010(3) 0.000(2) 0.002(2)
C14 0.017(2) 0.028(3) 0.021(3) 0.005(2) 0.001(2) -0.004(2)
C15 0.014(2) 0.019(3) 0.018(3) -0.001(2) 0.000(2) 0.000(2)
C16 0.012(2) 0.025(3) 0.012(3) -0.002(2) 0.001(2) -0.005(2)
C17 0.014(2) 0.020(3) 0.016(3) -0.003(2) 0.001(2) 0.000(2)
C18 0.018(2) 0.020(3) 0.028(3) -0.005(2) 0.002(2) 0.001(2)
C19 0.017(2) 0.021(3) 0.032(3) 0.003(2) -0.002(2) 0.005(2)
C20 0.019(2) 0.022(3) 0.020(3) 0.005(2) 0.000(2) -0.001(2)
C21 0.017(2) 0.020(3) 0.017(3) -0.001(2) 0.002(2) 0.001(2)
C22 0.014(2) 0.032(4) 0.019(3) -0.002(2) -0.002(2) -0.002(2)
C23 0.028(3) 0.029(4) 0.013(3) 0.001(2) 0.002(2) 0.000(2)
C24 0.022(3) 0.020(3) 0.018(3) 0.000(2) 0.006(2) -0.001(2)
C25 0.014(2) 0.028(3) 0.026(3) 0.000(3) 0.001(2) 0.000(2)
C26 0.017(2) 0.027(3) 0.016(3) -0.003(2) -0.001(2) -0.004(2)
C27 0.023(3) 0.037(4) 0.019(3) -0.001(3) 0.003(2) 0.001(2)
N1 0.018(2) 0.027(3) 0.021(3) -0.002(2) -0.0020(19) 0.000(2)
N2 0.016(2) 0.015(2) 0.018(2) 0.0017(18) -0.0016(17) 0.0021(16)
N3 0.0158(19) 0.017(2) 0.016(2) -0.0010(19) 0.0021(17) 0.0005(17)
N4 0.033(3) 0.062(4) 0.030(3) 0.003(3) 0.011(3) -0.006(3)
Pt1 0.01437(11) 0.01613(14) 0.01315(12) -0.00022(8) 0.00251(8) 0.00084(7)

_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
C1 C2 1.367(7) . ?
C1 N1 1.379(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.395(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.399(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.378(7) . ?
C5 C6 1.448(8) . ?
C6 C11 1.387(6) . ?
C6 C7 1.390(7) . ?
C7 C8 1.392(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.375(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.371(7) . ?
C10 H10 0.9300 . ?
C11 Pt1 2.021(5) . ?
C12 N2 1.340(7) . ?
C12 C13 1.403(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.362(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.424(7) . ?
C14 H14 0.9300 . ?
C15 N2 1.391(6) . ?
C15 C16 1.413(8) . ?
C16 C17 1.399(7) . ?
C16 C21 1.496(7) . ?
C17 N3 1.404(6) . ?
C17 C18 1.421(7) . ?
C18 C19 1.364(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.405(7) . ?
C19 H19 0.9300 . ?
C20 N3 1.329(7) . ?
C20 H20 0.9300 . ?
C21 C26 1.397(7) . ?
C21 C22 1.409(8) . ?
C22 C23 1.380(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.391(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.397(8) . ?
C24 C27 1.449(8) . ?
C25 C26 1.376(8) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 N4 1.132(8) . ?
N1 Pt1 2.027(4) . ?
N2 Pt1 2.045(4) . ?
N3 Pt1 2.047(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 122.4(5) . . ?
C2 C1 H1 118.8 . . ?
N1 C1 H1 118.8 . . ?
C1 C2 C3 119.6(6) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 119.0(5) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 120.0(5) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 120.6(5) . . ?
N1 C5 C6 114.3(4) . . ?
C4 C5 C6 124.8(5) . . ?
C11 C6 C7 120.7(5) . . ?
C11 C6 C5 114.5(4) . . ?
C7 C6 C5 124.5(5) . . ?
C6 C7 C8 120.1(5) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 119.0(5) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 119.8(5) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 122.2(5) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 C11 C6 117.6(4) . . ?
C10 C11 Pt1 129.1(4) . . ?
C6 C11 Pt1 113.3(3) . . ?
N2 C12 C13 111.9(5) . . ?
N2 C12 H12 124.0 . . ?
C13 C12 H12 124.0 . . ?
C14 C13 C12 106.6(5) . . ?
C14 C13 H13 126.7 . . ?
C12 C13 H13 126.7 . . ?
C13 C14 C15 106.8(5) . . ?
C13 C14 H14 126.6 . . ?
C15 C14 H14 126.6 . . ?
N2 C15 C16 123.6(5) . . ?
N2 C15 C14 109.2(5) . . ?
C16 C15 C14 125.7(5) . . ?
C17 C16 C15 125.2(5) . . ?
C17 C16 C21 117.9(5) . . ?
C15 C16 C21 116.0(5) . . ?
C16 C17 N3 123.3(5) . . ?
C16 C17 C18 127.6(4) . . ?
N3 C17 C18 108.2(5) . . ?
C19 C18 C17 107.6(5) . . ?
C19 C18 H18 126.2 . . ?
C17 C18 H18 126.2 . . ?
C18 C19 C20 105.9(5) . . ?
C18 C19 H19 127.0 . . ?
C20 C19 H19 127.0 . . ?
N3 C20 C19 112.5(5) . . ?
N3 C20 H20 123.8 . . ?
C19 C20 H20 123.8 . . ?
C26 C21 C22 118.3(5) . . ?
C26 C21 C16 119.3(5) . . ?
C22 C21 C16 122.2(5) . . ?
C23 C22 C21 120.5(5) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C24 119.8(5) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 120.6(5) . . ?
C23 C24 C27 122.1(5) . . ?
C25 C24 C27 117.3(5) . . ?
C26 C25 C24 119.1(5) . . ?
C26 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?
C25 C26 C21 121.6(6) . . ?
C25 C26 H26 119.2 . . ?
C21 C26 H26 119.2 . . ?
N4 C27 C24 175.8(7) . . ?
C5 N1 C1 118.1(4) . . ?
C5 N1 Pt1 113.3(4) . . ?
C1 N1 Pt1 128.5(4) . . ?
C12 N2 C15 105.5(4) . . ?
C12 N2 Pt1 128.8(4) . . ?
C15 N2 Pt1 125.3(3) . . ?
C20 N3 C17 105.7(4) . . ?
C20 N3 Pt1 128.3(3) . . ?
C17 N3 Pt1 125.0(3) . . ?
C11 Pt1 N1 79.66(19) . . ?
C11 Pt1 N2 177.20(17) . . ?
N1 Pt1 N2 97.65(17) . . ?
C11 Pt1 N3 96.57(18) . . ?
N1 Pt1 N3 175.41(17) . . ?
N2 Pt1 N3 86.08(16) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.269
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.319

#===END

###Material relevant to compound 8 at 173K ##

data_compound8
_database_code_depnum_ccdc_archive 'CCDC 729825'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H18 N4 Pd'
_chemical_formula_sum            'C27 H18 N4 Pd'
_chemical_formula_weight         504.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9990 1.0070 '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 '
_symmetry_space_group_name_Hall  '-P 2yn'

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                   15.0039(3)
_cell_length_b                   7.48110(10)
_cell_length_c                   18.2111(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3430(10)
_cell_angle_gamma                90.00
_cell_volume                     2035.24(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7914
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      29.84

_exptl_crystal_description       platelet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7415
_exptl_absorpt_correction_T_max  0.9289
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            25659
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         30.03
_reflns_number_total             5955
_reflns_number_gt                4922
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.3377P] 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    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5955
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.0883
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_restrained_S_all      1.204
_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
C1 C 0.19382(19) 0.1578(4) 0.33314(17) 0.0287(6) Uani 1 1 d . . .
H1 H 0.1550 0.2033 0.2949 0.034 Uiso 1 1 calc R . .
C2 C 0.1676(2) 0.1599(4) 0.40364(18) 0.0351(7) Uani 1 1 d . . .
H2 H 0.1118 0.2045 0.4126 0.042 Uiso 1 1 calc R . .
C3 C 0.2254(2) 0.0951(3) 0.46079(18) 0.0346(7) Uani 1 1 d . . .
H3 H 0.2085 0.0909 0.5086 0.041 Uiso 1 1 calc R . .
C4 C 0.3086(2) 0.0367(4) 0.44534(16) 0.0298(6) Uani 1 1 d . . .
H4 H 0.3492 -0.0033 0.4835 0.036 Uiso 1 1 calc R . .
C5 C 0.33248(18) 0.0368(3) 0.37371(15) 0.0238(5) Uani 1 1 d . . .
C6 C 0.42001(17) -0.0135(3) 0.35062(15) 0.0234(5) Uani 1 1 d . . .
C7 C 0.4866(2) -0.0959(3) 0.39678(17) 0.0289(6) Uani 1 1 d . . .
H7 H 0.4780 -0.1157 0.4461 0.035 Uiso 1 1 calc R . .
C8 C 0.5660(2) -0.1489(4) 0.36949(17) 0.0313(6) Uani 1 1 d . . .
H8 H 0.6113 -0.2014 0.4006 0.038 Uiso 1 1 calc R . .
C9 C 0.57705(19) -0.1229(3) 0.29617(18) 0.0297(6) Uani 1 1 d . . .
H9 H 0.6294 -0.1611 0.2774 0.036 Uiso 1 1 calc R . .
C10 C 0.51034(18) -0.0398(4) 0.24974(16) 0.0262(5) Uani 1 1 d . . .
H10 H 0.5188 -0.0246 0.2002 0.031 Uiso 1 1 calc R . .
C11 C 0.43137(16) 0.0210(3) 0.27582(14) 0.0210(5) Uani 1 1 d . . .
C12 C 0.12495(17) 0.0114(4) 0.16630(16) 0.0271(6) Uani 1 1 d . . .
H12 H 0.1107 0.0035 0.2148 0.033 Uiso 1 1 calc R . .
C13 C 0.06927(18) -0.0512(4) 0.10558(17) 0.0278(6) Uani 1 1 d . . .
H13 H 0.0136 -0.1051 0.1066 0.033 Uiso 1 1 calc R . .
C14 C 0.11326(16) -0.0170(3) 0.04467(15) 0.0235(5) Uani 1 1 d . . .
H14 H 0.0930 -0.0427 -0.0040 0.028 Uiso 1 1 calc R . .
C15 C 0.19614(16) 0.0655(3) 0.06995(15) 0.0203(5) Uani 1 1 d . . .
C16 C 0.26605(16) 0.1074(3) 0.02718(14) 0.0187(5) Uani 1 1 d . . .
C17 C 0.35166(16) 0.1667(3) 0.05329(14) 0.0201(5) Uani 1 1 d . . .
C18 C 0.41577(16) 0.2486(3) 0.01087(16) 0.0232(5) Uani 1 1 d . . .
H18 H 0.4119 0.2589 -0.0402 0.028 Uiso 1 1 calc R . .
C19 C 0.48434(17) 0.3096(4) 0.05982(16) 0.0259(5) Uani 1 1 d . . .
H19 H 0.5353 0.3706 0.0484 0.031 Uiso 1 1 calc R . .
C20 C 0.46248(17) 0.2618(3) 0.13002(15) 0.0246(5) Uani 1 1 d . . .
H20 H 0.4978 0.2876 0.1734 0.030 Uiso 1 1 calc R . .
C21 C 0.24705(17) 0.0883(3) -0.05423(15) 0.0204(5) Uani 1 1 d . . .
C22 C 0.17545(17) 0.1762(3) -0.09247(15) 0.0235(5) Uani 1 1 d . . .
H22 H 0.1405 0.2534 -0.0672 0.028 Uiso 1 1 calc R . .
C23 C 0.15541(17) 0.1510(4) -0.16715(15) 0.0242(5) Uani 1 1 d . . .
H23 H 0.1073 0.2107 -0.1920 0.029 Uiso 1 1 calc R . .
C24 C 0.20756(18) 0.0355(3) -0.20528(15) 0.0238(5) Uani 1 1 d . . .
C25 C 0.28047(18) -0.0508(4) -0.16782(16) 0.0260(6) Uani 1 1 d . . .
H25 H 0.3159 -0.1266 -0.1932 0.031 Uiso 1 1 calc R . .
C26 C 0.30025(17) -0.0241(3) -0.09318(15) 0.0240(5) Uani 1 1 d . . .
H26 H 0.3493 -0.0813 -0.0686 0.029 Uiso 1 1 calc R . .
C27 C 0.18542(19) 0.0051(4) -0.28279(17) 0.0304(6) Uani 1 1 d . . .
N1 N 0.27313(16) 0.0925(3) 0.31755(13) 0.0235(5) Uani 1 1 d . . .
N2 N 0.20054(15) 0.0834(3) 0.14680(13) 0.0222(5) Uani 1 1 d . . .
N3 N 0.38415(13) 0.1738(3) 0.12717(12) 0.0218(4) Uani 1 1 d . . .
N4 N 0.16818(19) -0.0174(4) -0.34461(15) 0.0425(7) Uani 1 1 d . . .
Pd1 Pd 0.321667(12) 0.10232(2) 0.216038(10) 0.02016(8) 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
C1 0.0322(14) 0.0254(12) 0.0289(16) 0.0015(11) 0.0057(12) 0.0012(11)
C2 0.0384(16) 0.0289(13) 0.0406(19) -0.0053(13) 0.0180(14) -0.0038(12)
C3 0.0479(19) 0.0302(14) 0.0279(17) -0.0047(11) 0.0161(14) -0.0088(12)
C4 0.0390(16) 0.0287(13) 0.0221(15) 0.0020(11) 0.0047(12) -0.0057(12)
C5 0.0298(13) 0.0208(11) 0.0209(14) 0.0008(9) 0.0021(10) -0.0056(10)
C6 0.0276(13) 0.0210(11) 0.0209(14) 0.0015(9) -0.0010(10) -0.0046(9)
C7 0.0365(16) 0.0295(13) 0.0193(15) 0.0049(10) -0.0047(12) -0.0052(11)
C8 0.0309(14) 0.0294(12) 0.0315(17) 0.0066(12) -0.0089(12) -0.0010(11)
C9 0.0234(13) 0.0284(13) 0.0372(18) 0.0052(11) 0.0018(12) 0.0007(10)
C10 0.0263(13) 0.0282(12) 0.0240(15) 0.0057(11) 0.0014(11) 0.0004(10)
C11 0.0222(12) 0.0217(11) 0.0182(13) 0.0029(9) -0.0028(9) -0.0029(9)
C12 0.0206(12) 0.0358(14) 0.0253(15) 0.0067(11) 0.0043(10) 0.0003(10)
C13 0.0191(12) 0.0315(13) 0.0327(17) 0.0051(12) 0.0019(11) -0.0036(10)
C14 0.0178(11) 0.0253(12) 0.0264(15) 0.0015(10) -0.0028(10) 0.0000(9)
C15 0.0192(11) 0.0213(10) 0.0200(13) 0.0022(9) -0.0003(10) 0.0028(9)
C16 0.0183(11) 0.0199(10) 0.0174(13) 0.0008(8) -0.0014(9) 0.0037(8)
C17 0.0195(11) 0.0232(11) 0.0175(13) 0.0040(9) 0.0011(9) 0.0008(9)
C18 0.0189(11) 0.0309(12) 0.0202(13) 0.0052(10) 0.0037(9) 0.0003(9)
C19 0.0187(11) 0.0316(13) 0.0279(15) 0.0072(11) 0.0047(10) -0.0020(10)
C20 0.0190(11) 0.0288(12) 0.0255(15) 0.0058(10) -0.0016(10) -0.0029(9)
C21 0.0185(11) 0.0230(11) 0.0195(13) 0.0018(9) 0.0008(10) -0.0009(9)
C22 0.0230(12) 0.0247(12) 0.0226(14) -0.0012(10) 0.0021(10) 0.0027(10)
C23 0.0212(12) 0.0288(12) 0.0224(14) 0.0015(10) 0.0012(10) 0.0010(10)
C24 0.0270(13) 0.0237(12) 0.0206(14) -0.0012(10) 0.0017(10) -0.0033(10)
C25 0.0261(13) 0.0262(12) 0.0264(15) -0.0031(10) 0.0061(11) 0.0026(10)
C26 0.0200(12) 0.0260(12) 0.0259(15) 0.0027(10) 0.0022(10) 0.0033(10)
C27 0.0331(15) 0.0312(13) 0.0265(16) -0.0012(11) 0.0002(12) 0.0022(11)
N1 0.0278(12) 0.0219(10) 0.0216(12) 0.0020(8) 0.0060(9) -0.0008(8)
N2 0.0181(10) 0.0291(11) 0.0194(12) 0.0045(8) 0.0022(8) 0.0006(8)
N3 0.0183(10) 0.0285(10) 0.0184(12) 0.0060(8) 0.0003(8) -0.0021(8)
N4 0.0495(16) 0.0476(15) 0.0290(16) -0.0048(12) -0.0035(13) 0.0102(13)
Pd1 0.01893(11) 0.02416(11) 0.01735(13) 0.00383(7) 0.00140(8) -0.00038(6)

_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
C1 N1 1.341(3) . ?
C1 C2 1.377(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.379(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9300 . ?
C5 N1 1.357(4) . ?
C5 C6 1.465(4) . ?
C6 C7 1.388(4) . ?
C6 C11 1.412(4) . ?
C7 C8 1.391(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.374(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.395(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.393(4) . ?
C10 H10 0.9300 . ?
C11 Pd1 1.983(2) . ?
C12 N2 1.333(3) . ?
C12 C13 1.403(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.367(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.426(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.399(3) . ?
C15 N2 1.401(3) . ?
C16 C17 1.400(3) . ?
C16 C21 1.490(4) . ?
C17 N3 1.389(3) . ?
C17 C18 1.427(3) . ?
C18 C19 1.375(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.396(4) . ?
C19 H19 0.9300 . ?
C20 N3 1.344(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.390(4) . ?
C21 C26 1.397(3) . ?
C22 C23 1.378(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.393(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.393(4) . ?
C24 C27 1.438(4) . ?
C25 C26 1.379(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 N4 1.144(4) . ?
N1 Pd1 2.050(2) . ?
N2 Pd1 2.118(2) . ?
N3 Pd1 2.017(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.5(3) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C1 C2 C3 119.0(3) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 118.4(3) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C5 120.8(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
N1 C5 C4 120.0(3) . . ?
N1 C5 C6 113.9(2) . . ?
C4 C5 C6 126.0(3) . . ?
C7 C6 C11 121.4(3) . . ?
C7 C6 C5 123.6(3) . . ?
C11 C6 C5 114.9(2) . . ?
C6 C7 C8 120.1(3) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 119.4(3) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 120.5(3) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C11 C10 C9 121.6(3) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C6 116.9(2) . . ?
C10 C11 Pd1 127.0(2) . . ?
C6 C11 Pd1 114.66(18) . . ?
N2 C12 C13 112.6(3) . . ?
N2 C12 H12 123.7 . . ?
C13 C12 H12 123.7 . . ?
C14 C13 C12 106.3(2) . . ?
C14 C13 H13 126.9 . . ?
C12 C13 H13 126.9 . . ?
C13 C14 C15 107.0(2) . . ?
C13 C14 H14 126.5 . . ?
C15 C14 H14 126.5 . . ?
C16 C15 N2 124.5(2) . . ?
C16 C15 C14 126.4(2) . . ?
N2 C15 C14 108.8(2) . . ?
C15 C16 C17 126.4(2) . . ?
C15 C16 C21 116.6(2) . . ?
C17 C16 C21 116.9(2) . . ?
N3 C17 C16 124.7(2) . . ?
N3 C17 C18 108.3(2) . . ?
C16 C17 C18 126.6(2) . . ?
C19 C18 C17 107.0(2) . . ?
C19 C18 H18 126.5 . . ?
C17 C18 H18 126.5 . . ?
C18 C19 C20 106.5(2) . . ?
C18 C19 H19 126.8 . . ?
C20 C19 H19 126.8 . . ?
N3 C20 C19 111.7(2) . . ?
N3 C20 H20 124.2 . . ?
C19 C20 H20 124.2 . . ?
C22 C21 C26 118.8(2) . . ?
C22 C21 C16 121.3(2) . . ?
C26 C21 C16 119.8(2) . . ?
C23 C22 C21 121.1(2) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C22 C23 C24 119.7(2) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 119.7(2) . . ?
C25 C24 C27 120.4(2) . . ?
C23 C24 C27 119.9(3) . . ?
C26 C25 C24 120.2(2) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C21 120.5(2) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
N4 C27 C24 179.3(3) . . ?
C1 N1 C5 119.0(2) . . ?
C1 N1 Pd1 125.1(2) . . ?
C5 N1 Pd1 115.29(18) . . ?
C12 N2 C15 105.4(2) . . ?
C12 N2 Pd1 124.92(19) . . ?
C15 N2 Pd1 123.98(17) . . ?
C20 N3 C17 106.4(2) . . ?
C20 N3 Pd1 124.69(19) . . ?
C17 N3 Pd1 128.31(16) . . ?
C11 Pd1 N3 95.61(9) . . ?
C11 Pd1 N1 80.81(10) . . ?
N3 Pd1 N1 164.54(9) . . ?
C11 Pd1 N2 158.27(9) . . ?
N3 Pd1 N2 88.69(8) . . ?
N1 Pd1 N2 100.21(9) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.682
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.217

#===END