# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Jose Lassaletta'
'Manuel Alcarazo'
'Eleuterio Alvarez'
'Elena Diez'
'Rosario Fernandez'
'Javier Iglesias-Siguenza'
'Abel Ros'

_publ_contact_author_name        'Jose Lassaletta'
_publ_contact_author_email       JMLASSA@IIQ.CSIC.ES

_publ_section_title              
;
Synthesis, structure and properties of
[1,2,4]triazolo[4,3-a]pyridin-3-ylidene Rhodium and
Palladium complexes
;

# Attachment '10.cif'

#=========================================================================
# Data for compound 10 (local labelling ea11005a)
#=========================================================================

data_10
_database_code_depnum_ccdc_archive 'CCDC 727062'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H23 Cl N3 Rh'
_chemical_formula_sum            'C21 H23 Cl N3 Rh'
_chemical_formula_weight         455.78

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/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                   23.5474(17)
_cell_length_b                   16.3564(12)
_cell_length_c                   9.7329(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.310(3)
_cell_angle_gamma                90.00
_cell_volume                     3747.7(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8725
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      30.57

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6843
_exptl_absorpt_correction_T_max  0.7744
_exptl_absorpt_process_details   
;
SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
X-ray Solutions, Madison, Wisconsin, USA.
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Bruker-Nonius X8kappa APEX II CCD area detector'
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_decay_%        0
_diffrn_reflns_number            39366
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         30.66
_reflns_number_total             5734
_reflns_number_gt                5306
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.1264P)^2^+2.7047P] 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     SHELXL
_refine_ls_extinction_coef       0.0028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5734
_refine_ls_number_parameters     236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1781
_refine_ls_wR_factor_gt          0.1544
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
Rh1 Rh 0.63079(3) 0.18959(4) 0.12054(8) 0.0150(3) Uani 1 1 d . . .
Cl1 Cl 0.66339(11) 0.20476(17) -0.1086(3) 0.0216(5) Uani 1 1 d . . .
N1 N 0.5772(4) 0.3581(5) 0.1099(9) 0.0167(15) Uani 1 1 d . . .
N2 N 0.5354(4) 0.4084(6) 0.0578(10) 0.0211(17) Uani 1 1 d . . .
N3 N 0.5229(4) 0.2780(6) -0.0021(9) 0.0199(16) Uani 1 1 d . . .
C1 C 0.5721(4) 0.2783(6) 0.0771(10) 0.0179(18) Uani 1 1 d . . .
C2 C 0.5020(5) 0.3580(7) -0.0118(11) 0.0223(19) Uani 1 1 d . . .
C3 C 0.4516(4) 0.3752(7) -0.0886(12) 0.0215(19) Uani 1 1 d . . .
H3 H 0.4377 0.4294 -0.0978 0.026 Uiso 1 1 d R . .
C4 C 0.4243(5) 0.3118(7) -0.1478(12) 0.024(2) Uani 1 1 d . . .
H4 H 0.3908 0.3221 -0.2012 0.029 Uiso 1 1 d R . .
C5 C 0.4436(4) 0.2301(7) -0.1337(11) 0.0211(19) Uani 1 1 d . . .
H5 H 0.4217 0.1870 -0.1731 0.025 Uiso 1 1 d R . .
C6 C 0.4931(5) 0.2123(7) -0.0644(10) 0.0198(18) Uani 1 1 d . . .
C7 C 0.5174(5) 0.1286(6) -0.0526(12) 0.023(2) Uani 1 1 d . . .
H7A H 0.4916 0.0895 -0.0976 0.034 Uiso 1 1 d R . .
H7B H 0.5224 0.1142 0.0447 0.034 Uiso 1 1 d R . .
H7C H 0.5543 0.1271 -0.0971 0.034 Uiso 1 1 d R . .
C8 C 0.6213(4) 0.3940(6) 0.1946(11) 0.0189(18) Uani 1 1 d . . .
C9 C 0.6774(4) 0.3731(6) 0.1778(12) 0.0214(19) Uani 1 1 d . . .
H9 H 0.6881 0.3365 0.1070 0.026 Uiso 1 1 d R . .
C10 C 0.7184(5) 0.4067(8) 0.2672(14) 0.029(2) Uani 1 1 d . . .
H10 H 0.7572 0.3918 0.2593 0.034 Uiso 1 1 d R . .
C11 C 0.7026(5) 0.4620(8) 0.3678(13) 0.027(2) Uani 1 1 d . . .
H11 H 0.7304 0.4841 0.4294 0.032 Uiso 1 1 d R . .
C12 C 0.6457(5) 0.4851(7) 0.3781(12) 0.025(2) Uani 1 1 d . . .
H12 H 0.6351 0.5248 0.4440 0.030 Uiso 1 1 d R . .
C13 C 0.6049(5) 0.4503(7) 0.2931(12) 0.0219(19) Uani 1 1 d . . .
H13 H 0.5660 0.4646 0.3017 0.026 Uiso 1 1 d R . .
C14 C 0.7123(5) 0.1348(8) 0.1779(13) 0.028(2) Uani 1 1 d . . .
H14 H 0.7285 0.1616 0.1016 0.034 Uiso 1 1 d R . .
C15 C 0.6746(5) 0.0726(7) 0.1470(13) 0.026(2) Uani 1 1 d . . .
H15 H 0.6648 0.0621 0.0534 0.031 Uiso 1 1 d R . .
C16 C 0.6486(7) 0.0210(9) 0.2567(17) 0.040(3) Uani 1 1 d . . .
H16A H 0.6753 0.0178 0.3365 0.048 Uiso 1 1 d R . .
H16B H 0.6429 -0.0351 0.2209 0.048 Uiso 1 1 d R . .
C17 C 0.5914(6) 0.0543(7) 0.3049(15) 0.033(3) Uani 1 1 d . . .
H17A H 0.5604 0.0276 0.2512 0.039 Uiso 1 1 d R . .
H17B H 0.5868 0.0396 0.4027 0.039 Uiso 1 1 d R . .
C18 C 0.5857(5) 0.1462(7) 0.2898(12) 0.023(2) Uani 1 1 d . . .
H18 H 0.5523 0.1664 0.2450 0.028 Uiso 1 1 d R . .
C19 C 0.6255(4) 0.2034(7) 0.3363(12) 0.0204(19) Uani 1 1 d . . .
H19 H 0.6178 0.2596 0.3201 0.025 Uiso 1 1 d R . .
C20 C 0.6812(5) 0.1809(9) 0.4123(13) 0.031(3) Uani 1 1 d . . .
H20A H 0.6915 0.2257 0.4766 0.037 Uiso 1 1 d R . .
H20B H 0.6748 0.1311 0.4677 0.037 Uiso 1 1 d R . .
C21 C 0.7311(6) 0.1656(10) 0.3183(15) 0.037(3) Uani 1 1 d . . .
H21A H 0.7526 0.2171 0.3074 0.044 Uiso 1 1 d R . .
H21B H 0.7569 0.1249 0.3618 0.044 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
Rh1 0.0107(4) 0.0120(4) 0.0222(4) 0.0002(2) -0.0002(2) 0.0023(2)
Cl1 0.0156(10) 0.0252(12) 0.0242(11) 0.0002(9) 0.0022(8) 0.0046(9)
N1 0.011(3) 0.013(4) 0.025(4) 0.000(3) 0.000(3) -0.001(3)
N2 0.018(4) 0.017(4) 0.028(4) 0.000(3) -0.004(3) 0.004(3)
N3 0.022(4) 0.018(4) 0.019(4) -0.001(3) 0.000(3) -0.001(3)
C1 0.020(4) 0.015(4) 0.018(4) 0.000(3) 0.002(3) 0.005(3)
C2 0.024(5) 0.022(5) 0.021(5) 0.000(4) 0.000(4) 0.003(4)
C3 0.015(4) 0.019(5) 0.030(5) 0.001(4) -0.003(4) 0.002(4)
C4 0.016(5) 0.030(6) 0.025(5) -0.001(4) -0.001(4) 0.006(4)
C5 0.016(4) 0.023(5) 0.025(5) -0.003(4) -0.002(3) 0.004(4)
C6 0.019(5) 0.022(5) 0.019(4) -0.002(3) 0.000(3) 0.000(4)
C7 0.026(5) 0.014(4) 0.028(5) -0.003(4) -0.001(4) 0.002(4)
C8 0.017(4) 0.015(4) 0.024(5) 0.000(3) -0.001(3) -0.003(3)
C9 0.015(4) 0.016(4) 0.033(5) 0.001(4) 0.003(4) -0.002(3)
C10 0.019(5) 0.029(6) 0.039(6) 0.000(5) 0.002(4) -0.003(4)
C11 0.017(5) 0.027(5) 0.037(6) -0.003(4) -0.002(4) -0.006(4)
C12 0.021(5) 0.024(5) 0.031(6) -0.006(4) 0.002(4) -0.006(4)
C13 0.019(5) 0.018(4) 0.029(5) -0.003(4) 0.002(4) -0.004(4)
C14 0.023(5) 0.027(5) 0.034(6) 0.001(4) -0.005(4) 0.012(4)
C15 0.026(5) 0.016(5) 0.036(6) 0.002(4) 0.003(4) 0.014(4)
C16 0.041(8) 0.026(6) 0.053(9) 0.009(6) 0.011(6) 0.008(5)
C17 0.033(6) 0.017(5) 0.048(7) 0.008(5) 0.002(5) -0.001(4)
C18 0.019(5) 0.024(5) 0.027(5) 0.005(4) -0.001(4) 0.000(4)
C19 0.010(4) 0.019(4) 0.033(5) 0.007(4) 0.003(3) 0.003(3)
C20 0.018(5) 0.048(8) 0.026(5) 0.001(5) -0.002(4) -0.006(5)
C21 0.026(6) 0.046(8) 0.037(7) 0.001(6) -0.009(5) 0.012(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
Rh1 C1 2.041(10) . ?
Rh1 C18 2.104(11) . ?
Rh1 C19 2.119(12) . ?
Rh1 C14 2.180(11) . ?
Rh1 C15 2.186(10) . ?
Rh1 Cl1 2.388(3) . ?
N1 C1 1.349(13) . ?
N1 N2 1.370(12) . ?
N1 C8 1.437(13) . ?
N2 C2 1.317(14) . ?
N3 C1 1.377(14) . ?
N3 C2 1.400(14) . ?
N3 C6 1.412(14) . ?
C2 C3 1.414(15) . ?
C3 C4 1.344(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.416(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.365(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.486(15) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.380(14) . ?
C8 C13 1.390(15) . ?
C9 C10 1.397(16) . ?
C9 H9 0.9500 . ?
C10 C11 1.389(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.398(16) . ?
C11 H11 0.9500 . ?
C12 C13 1.375(15) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.379(18) . ?
C14 C21 1.512(19) . ?
C14 H14 0.9500 . ?
C15 C16 1.503(18) . ?
C15 H15 0.9500 . ?
C16 C17 1.54(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.515(16) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.394(16) . ?
C18 H18 0.9500 . ?
C19 C20 1.535(16) . ?
C19 H19 0.9500 . ?
C20 C21 1.526(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 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
C1 Rh1 C18 92.9(4) . . ?
C1 Rh1 C19 94.3(4) . . ?
C18 Rh1 C19 38.5(4) . . ?
C1 Rh1 C14 159.0(5) . . ?
C18 Rh1 C14 96.8(5) . . ?
C19 Rh1 C14 82.0(4) . . ?
C1 Rh1 C15 164.1(5) . . ?
C18 Rh1 C15 81.8(5) . . ?
C19 Rh1 C15 90.8(4) . . ?
C14 Rh1 C15 36.8(5) . . ?
C1 Rh1 Cl1 87.9(3) . . ?
C18 Rh1 Cl1 160.9(3) . . ?
C19 Rh1 Cl1 160.4(3) . . ?
C14 Rh1 Cl1 89.0(4) . . ?
C15 Rh1 Cl1 92.3(3) . . ?
C1 N1 N2 115.8(8) . . ?
C1 N1 C8 126.2(9) . . ?
N2 N1 C8 118.0(8) . . ?
C2 N2 N1 103.3(9) . . ?
C1 N3 C2 109.0(9) . . ?
C1 N3 C6 130.2(9) . . ?
C2 N3 C6 120.8(9) . . ?
N1 C1 N3 101.8(8) . . ?
N1 C1 Rh1 125.6(8) . . ?
N3 C1 Rh1 132.2(8) . . ?
N2 C2 N3 110.2(10) . . ?
N2 C2 C3 129.1(10) . . ?
N3 C2 C3 120.7(10) . . ?
C4 C3 C2 117.4(10) . . ?
C4 C3 H3 121.3 . . ?
C2 C3 H3 121.3 . . ?
C3 C4 C5 122.4(10) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C6 C5 C4 121.2(10) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 N3 117.3(10) . . ?
C5 C6 C7 123.9(10) . . ?
N3 C6 C7 118.8(9) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C13 121.9(10) . . ?
C9 C8 N1 120.8(9) . . ?
C13 C8 N1 117.3(9) . . ?
C8 C9 C10 118.6(10) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 120.2(11) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 119.9(11) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.1(11) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C8 119.2(10) . . ?
C12 C13 H13 120.4 . . ?
C8 C13 H13 120.4 . . ?
C15 C14 C21 128.0(13) . . ?
C15 C14 Rh1 71.8(7) . . ?
C21 C14 Rh1 109.4(8) . . ?
C15 C14 H14 116.0 . . ?
C21 C14 H14 116.0 . . ?
Rh1 C14 H14 88.7 . . ?
C14 C15 C16 122.0(13) . . ?
C14 C15 Rh1 71.4(6) . . ?
C16 C15 Rh1 112.1(8) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
Rh1 C15 H15 86.7 . . ?
C15 C16 C17 113.1(11) . . ?
C15 C16 H16A 109.0 . . ?
C17 C16 H16A 109.0 . . ?
C15 C16 H16B 109.0 . . ?
C17 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C18 C17 C16 113.5(11) . . ?
C18 C17 H17A 108.9 . . ?
C16 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
C16 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C19 C18 C17 125.2(11) . . ?
C19 C18 Rh1 71.3(6) . . ?
C17 C18 Rh1 111.5(8) . . ?
C19 C18 H18 117.4 . . ?
C17 C18 H18 117.4 . . ?
Rh1 C18 H18 87.2 . . ?
C18 C19 C20 123.8(10) . . ?
C18 C19 Rh1 70.1(7) . . ?
C20 C19 Rh1 112.5(7) . . ?
C18 C19 H19 118.1 . . ?
C20 C19 H19 118.1 . . ?
Rh1 C19 H19 87.3 . . ?
C21 C20 C19 114.3(10) . . ?
C21 C20 H20A 108.7 . . ?
C19 C20 H20A 108.7 . . ?
C21 C20 H20B 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C14 C21 C20 112.5(11) . . ?
C14 C21 H21A 109.1 . . ?
C20 C21 H21A 109.1 . . ?
C14 C21 H21B 109.1 . . ?
C20 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?

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
C1 N1 N2 C2 -0.1(12) . . . . ?
C8 N1 N2 C2 -179.2(9) . . . . ?
N2 N1 C1 N3 -0.1(11) . . . . ?
C8 N1 C1 N3 178.9(9) . . . . ?
N2 N1 C1 Rh1 173.2(7) . . . . ?
C8 N1 C1 Rh1 -7.7(15) . . . . ?
C2 N3 C1 N1 0.3(11) . . . . ?
C6 N3 C1 N1 -177.5(10) . . . . ?
C2 N3 C1 Rh1 -172.4(8) . . . . ?
C6 N3 C1 Rh1 9.7(17) . . . . ?
C18 Rh1 C1 N1 101.1(9) . . . . ?
C19 Rh1 C1 N1 62.5(9) . . . . ?
C14 Rh1 C1 N1 -16.4(18) . . . . ?
C15 Rh1 C1 N1 171.0(13) . . . . ?
Cl1 Rh1 C1 N1 -98.0(9) . . . . ?
C18 Rh1 C1 N3 -87.7(10) . . . . ?
C19 Rh1 C1 N3 -126.3(10) . . . . ?
C14 Rh1 C1 N3 154.9(12) . . . . ?
C15 Rh1 C1 N3 -18(2) . . . . ?
Cl1 Rh1 C1 N3 73.2(10) . . . . ?
N1 N2 C2 N3 0.2(12) . . . . ?
N1 N2 C2 C3 -179.8(11) . . . . ?
C1 N3 C2 N2 -0.4(13) . . . . ?
C6 N3 C2 N2 177.7(9) . . . . ?
C1 N3 C2 C3 179.6(10) . . . . ?
C6 N3 C2 C3 -2.3(16) . . . . ?
N2 C2 C3 C4 -178.3(12) . . . . ?
N3 C2 C3 C4 1.7(17) . . . . ?
C2 C3 C4 C5 1.1(17) . . . . ?
C3 C4 C5 C6 -3.6(18) . . . . ?
C4 C5 C6 N3 2.9(16) . . . . ?
C4 C5 C6 C7 -176.4(10) . . . . ?
C1 N3 C6 C5 177.5(10) . . . . ?
C2 N3 C6 C5 -0.1(15) . . . . ?
C1 N3 C6 C7 -3.1(16) . . . . ?
C2 N3 C6 C7 179.2(10) . . . . ?
C1 N1 C8 C9 44.8(15) . . . . ?
N2 N1 C8 C9 -136.1(10) . . . . ?
C1 N1 C8 C13 -135.2(11) . . . . ?
N2 N1 C8 C13 43.8(13) . . . . ?
C13 C8 C9 C10 3.1(16) . . . . ?
N1 C8 C9 C10 -176.9(10) . . . . ?
C8 C9 C10 C11 -2.0(18) . . . . ?
C9 C10 C11 C12 -1.0(19) . . . . ?
C10 C11 C12 C13 3.0(19) . . . . ?
C11 C12 C13 C8 -1.9(18) . . . . ?
C9 C8 C13 C12 -1.2(17) . . . . ?
N1 C8 C13 C12 178.8(10) . . . . ?
C1 Rh1 C14 C15 -176.6(10) . . . . ?
C18 Rh1 C14 C15 66.6(8) . . . . ?
C19 Rh1 C14 C15 102.3(8) . . . . ?
Cl1 Rh1 C14 C15 -95.2(7) . . . . ?
C1 Rh1 C14 C21 58.5(17) . . . . ?
C18 Rh1 C14 C21 -58.3(10) . . . . ?
C19 Rh1 C14 C21 -22.6(10) . . . . ?
C15 Rh1 C14 C21 -124.9(14) . . . . ?
Cl1 Rh1 C14 C21 139.9(10) . . . . ?
C21 C14 C15 C16 -4.1(18) . . . . ?
Rh1 C14 C15 C16 -104.9(11) . . . . ?
C21 C14 C15 Rh1 100.8(12) . . . . ?
C1 Rh1 C15 C14 175.6(14) . . . . ?
C18 Rh1 C15 C14 -113.0(8) . . . . ?
C19 Rh1 C15 C14 -75.4(8) . . . . ?
Cl1 Rh1 C15 C14 85.2(7) . . . . ?
C1 Rh1 C15 C16 -67(2) . . . . ?
C18 Rh1 C15 C16 4.8(10) . . . . ?
C19 Rh1 C15 C16 42.4(11) . . . . ?
C14 Rh1 C15 C16 117.8(14) . . . . ?
Cl1 Rh1 C15 C16 -157.0(10) . . . . ?
C14 C15 C16 C17 92.1(16) . . . . ?
Rh1 C15 C16 C17 10.9(16) . . . . ?
C15 C16 C17 C18 -27.9(19) . . . . ?
C16 C17 C18 C19 -50.1(18) . . . . ?
C16 C17 C18 Rh1 31.6(15) . . . . ?
C1 Rh1 C18 C19 -93.3(7) . . . . ?
C14 Rh1 C18 C19 68.0(7) . . . . ?
C15 Rh1 C18 C19 101.8(7) . . . . ?
Cl1 Rh1 C18 C19 174.8(7) . . . . ?
C1 Rh1 C18 C17 145.3(9) . . . . ?
C19 Rh1 C18 C17 -121.4(11) . . . . ?
C14 Rh1 C18 C17 -53.4(9) . . . . ?
C15 Rh1 C18 C17 -19.6(9) . . . . ?
Cl1 Rh1 C18 C17 53.4(15) . . . . ?
C17 C18 C19 C20 -0.9(19) . . . . ?
Rh1 C18 C19 C20 -104.4(11) . . . . ?
C17 C18 C19 Rh1 103.5(12) . . . . ?
C1 Rh1 C19 C18 89.2(7) . . . . ?
C14 Rh1 C19 C18 -111.6(7) . . . . ?
C15 Rh1 C19 C18 -75.7(7) . . . . ?
Cl1 Rh1 C19 C18 -174.9(7) . . . . ?
C1 Rh1 C19 C20 -151.4(9) . . . . ?
C18 Rh1 C19 C20 119.4(11) . . . . ?
C14 Rh1 C19 C20 7.8(9) . . . . ?
C15 Rh1 C19 C20 43.7(9) . . . . ?
Cl1 Rh1 C19 C20 -55.5(14) . . . . ?
C18 C19 C20 C21 89.1(15) . . . . ?
Rh1 C19 C20 C21 8.5(15) . . . . ?
C15 C14 C21 C20 -48.2(18) . . . . ?
Rh1 C14 C21 C20 33.5(15) . . . . ?
C19 C20 C21 C14 -28.3(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        30.66
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.795
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.413

###END

# Attachment '11.cif'

#=========================================================================
# Data for compound 11 (local labelling ea00407a)
#=========================================================================

data_11
_database_code_depnum_ccdc_archive 'CCDC 727063'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H23 Cl N3 Rh, C H2 Cl2'
_chemical_formula_sum            'C25 H25 Cl3 N3 Rh'
_chemical_formula_weight         576.74

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_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'
'-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                   11.2461(5)
_cell_length_b                   20.3332(9)
_cell_length_c                   20.7475(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4744.3(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6572
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      30.51

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2336
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5412
_exptl_absorpt_correction_T_max  0.7898
_exptl_absorpt_process_details   
;
SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
X-ray Solutions, Madison, Wisconsin, USA.
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Bruker-Nonius X8kappa APEX II CCD area detector'
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_decay_%        0
_diffrn_reflns_number            32732
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         30.51
_reflns_number_total             7229
_reflns_number_gt                5920
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker (2006). APEX 2. Version 2.1.'
_computing_cell_refinement       'Bruker (2006). APEX 2. Version 2.1.'
_computing_data_reduction        'Bruker (2006). APEX 2. Version 2.1.'
_computing_structure_solution    'Bruker (2006). APEX 2. Version 2.1.'
_computing_structure_refinement  'XL, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL v. 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. 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^)+(0.0649P)^2^+19.7429P] 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         7229
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1397
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_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
Rh1 Rh 0.11339(2) 0.138168(11) 0.556264(11) 0.01157(8) Uani 1 1 d . . .
Cl1 Cl 0.30098(7) 0.16824(4) 0.60216(4) 0.01894(16) Uani 1 1 d . . .
N1 N 0.1357(2) 0.00905(13) 0.62719(12) 0.0143(5) Uani 1 1 d . . .
N2 N 0.1964(2) -0.04970(13) 0.63315(13) 0.0159(5) Uani 1 1 d . . .
N3 N 0.2459(2) 0.00525(13) 0.54431(12) 0.0135(5) Uani 1 1 d . . .
C1 C 0.1629(3) 0.04460(15) 0.57459(14) 0.0135(5) Uani 1 1 d . . .
C2 C 0.2636(3) -0.05080(15) 0.58156(15) 0.0154(6) Uani 1 1 d . . .
C3 C 0.3467(3) -0.09977(16) 0.56161(16) 0.0189(6) Uani 1 1 d . . .
H3 H 0.3615 -0.1372 0.5879 0.023 Uiso 1 1 calc R . .
C4 C 0.4037(3) -0.09224(17) 0.50510(17) 0.0194(6) Uani 1 1 d . . .
H4 H 0.4600 -0.1244 0.4919 0.023 Uiso 1 1 calc R . .
C5 C 0.3809(3) -0.03619(16) 0.46414(16) 0.0163(6) Uani 1 1 d . . .
C6 C 0.3027(3) 0.01398(15) 0.48408(14) 0.0141(5) Uani 1 1 d . . .
C7 C 0.2815(3) 0.06894(17) 0.44545(15) 0.0173(6) Uani 1 1 d . . .
H7 H 0.2307 0.1032 0.4600 0.021 Uiso 1 1 calc R . .
C8 C 0.3360(3) 0.07275(18) 0.38539(16) 0.0220(7) Uani 1 1 d . . .
H8 H 0.3212 0.1096 0.3585 0.026 Uiso 1 1 calc R . .
C9 C 0.4122(3) 0.0231(2) 0.36423(17) 0.0243(7) Uani 1 1 d . . .
H9 H 0.4481 0.0261 0.3229 0.029 Uiso 1 1 calc R . .
C10 C 0.4352(3) -0.03010(18) 0.40298(16) 0.0208(7) Uani 1 1 d . . .
H10 H 0.4884 -0.0633 0.3885 0.025 Uiso 1 1 calc R . .
C11 C 0.0483(3) 0.02576(16) 0.67499(14) 0.0154(6) Uani 1 1 d . . .
C12 C 0.0533(3) 0.08689(16) 0.70503(15) 0.0176(6) Uani 1 1 d . . .
H12 H 0.1150 0.1172 0.6952 0.021 Uiso 1 1 calc R . .
C13 C -0.0344(3) 0.10257(18) 0.74986(16) 0.0219(6) Uani 1 1 d . . .
H13 H -0.0326 0.1440 0.7710 0.026 Uiso 1 1 calc R . .
C14 C -0.1242(3) 0.0581(2) 0.76373(17) 0.0230(7) Uani 1 1 d . . .
H14 H -0.1837 0.0693 0.7943 0.028 Uiso 1 1 calc R . .
C15 C -0.1280(3) -0.0026(2) 0.73340(17) 0.0246(7) Uani 1 1 d . . .
H15 H -0.1899 -0.0328 0.7432 0.030 Uiso 1 1 calc R . .
C16 C -0.0410(3) -0.01926(18) 0.68855(15) 0.0204(6) Uani 1 1 d . . .
H16 H -0.0427 -0.0608 0.6676 0.024 Uiso 1 1 calc R . .
C17 C -0.0190(3) 0.11598(15) 0.48653(15) 0.0156(6) Uani 1 1 d . . .
H17 H 0.0309 0.0809 0.4731 0.019 Uiso 1 1 calc R . .
C18 C -0.0398(3) 0.17224(16) 0.43936(15) 0.0180(6) Uani 1 1 d . . .
H18A H -0.1188 0.1918 0.4478 0.022 Uiso 1 1 calc R . .
H18B H -0.0404 0.1545 0.3949 0.022 Uiso 1 1 calc R . .
C19 C 0.0557(3) 0.22650(17) 0.44409(15) 0.0184(6) Uani 1 1 d . . .
H19A H 0.1225 0.2153 0.4151 0.022 Uiso 1 1 calc R . .
H19B H 0.0211 0.2686 0.4291 0.022 Uiso 1 1 calc R . .
C20 C 0.1029(3) 0.23546(15) 0.51163(16) 0.0161(6) Uani 1 1 d . . .
H20 H 0.1865 0.2402 0.5161 0.019 Uiso 1 1 calc R . .
C21 C 0.0361(3) 0.23739(15) 0.56766(16) 0.0162(6) Uani 1 1 d . . .
H21 H 0.0770 0.2404 0.6076 0.019 Uiso 1 1 calc R . .
C22 C -0.0987(3) 0.23500(17) 0.56901(17) 0.0185(6) Uani 1 1 d . . .
H22A H -0.1301 0.2517 0.5276 0.022 Uiso 1 1 calc R . .
H22B H -0.1282 0.2641 0.6037 0.022 Uiso 1 1 calc R . .
C23 C -0.1453(3) 0.16516(17) 0.58026(16) 0.0179(6) Uani 1 1 d . . .
H23A H -0.1491 0.1568 0.6272 0.021 Uiso 1 1 calc R . .
H23B H -0.2272 0.1620 0.5630 0.021 Uiso 1 1 calc R . .
C24 C -0.0691(3) 0.11248(16) 0.54894(15) 0.0161(6) Uani 1 1 d . . .
H24 H -0.0537 0.0739 0.5734 0.019 Uiso 1 1 calc R . .
Cl2 Cl 0.0630(4) 0.80788(16) 0.75140(12) 0.1342(12) Uani 1 1 d . . .
Cl3 Cl 0.2896(4) 0.7623(3) 0.77259(14) 0.222(3) Uani 1 1 d . . .
C25 C 0.2091(9) 0.8067(5) 0.7170(3) 0.107(4) Uani 1 1 d . . .
H25A H 0.2090 0.7847 0.6744 0.128 Uiso 1 1 calc R . .
H25B H 0.2411 0.8517 0.7122 0.128 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
Rh1 0.01139(13) 0.00894(12) 0.01437(12) 0.00010(7) -0.00084(7) -0.00008(8)
Cl1 0.0159(3) 0.0181(3) 0.0228(4) 0.0027(3) -0.0046(3) -0.0034(3)
N1 0.0165(12) 0.0124(12) 0.0141(11) -0.0005(9) -0.0009(9) 0.0014(10)
N2 0.0183(13) 0.0121(12) 0.0173(12) 0.0006(9) -0.0026(10) 0.0021(10)
N3 0.0137(11) 0.0107(11) 0.0160(11) 0.0001(9) 0.0002(9) 0.0001(9)
C1 0.0130(13) 0.0123(13) 0.0152(12) 0.0004(10) -0.0013(10) -0.0009(11)
C2 0.0188(15) 0.0102(13) 0.0172(13) -0.0003(10) -0.0038(11) 0.0000(11)
C3 0.0187(15) 0.0127(14) 0.0253(16) -0.0009(11) -0.0026(12) 0.0026(12)
C4 0.0182(15) 0.0142(14) 0.0258(16) -0.0053(12) -0.0021(12) 0.0032(12)
C5 0.0156(14) 0.0157(14) 0.0176(13) -0.0045(11) -0.0009(11) 0.0004(11)
C6 0.0142(13) 0.0134(13) 0.0148(13) -0.0030(10) 0.0001(10) 0.0002(11)
C7 0.0184(15) 0.0170(14) 0.0166(14) 0.0001(11) 0.0017(11) 0.0011(12)
C8 0.0232(17) 0.0250(17) 0.0178(14) 0.0030(12) 0.0012(12) -0.0002(14)
C9 0.0235(17) 0.0319(19) 0.0176(15) -0.0047(13) 0.0046(12) -0.0012(15)
C10 0.0187(15) 0.0224(16) 0.0215(15) -0.0086(12) 0.0035(12) 0.0010(13)
C11 0.0159(14) 0.0175(14) 0.0128(12) 0.0012(10) 0.0001(10) 0.0007(11)
C12 0.0200(15) 0.0153(14) 0.0177(14) 0.0000(11) 0.0010(11) 0.0010(12)
C13 0.0240(16) 0.0235(16) 0.0182(14) -0.0016(12) 0.0000(12) 0.0054(14)
C14 0.0179(16) 0.034(2) 0.0174(14) -0.0007(13) 0.0023(11) 0.0057(14)
C15 0.0186(16) 0.038(2) 0.0175(15) 0.0020(14) 0.0010(12) -0.0056(14)
C16 0.0220(16) 0.0239(16) 0.0153(14) -0.0007(12) -0.0005(11) -0.0037(13)
C17 0.0167(14) 0.0113(13) 0.0187(14) -0.0018(11) -0.0044(11) -0.0011(11)
C18 0.0202(15) 0.0149(14) 0.0187(14) 0.0009(11) -0.0043(11) -0.0008(12)
C19 0.0210(16) 0.0159(14) 0.0183(14) 0.0036(11) -0.0009(11) 0.0000(12)
C20 0.0157(14) 0.0108(13) 0.0219(14) 0.0024(11) -0.0018(11) -0.0006(11)
C21 0.0163(14) 0.0097(13) 0.0226(14) -0.0024(11) -0.0031(11) 0.0012(11)
C22 0.0169(15) 0.0151(15) 0.0234(15) -0.0011(12) 0.0000(12) 0.0045(12)
C23 0.0142(14) 0.0201(15) 0.0194(14) -0.0001(12) 0.0001(11) -0.0002(12)
C24 0.0136(14) 0.0141(14) 0.0207(14) 0.0018(11) -0.0030(11) -0.0016(11)
Cl2 0.203(4) 0.135(2) 0.0647(13) 0.0226(15) -0.0223(18) -0.039(2)
Cl3 0.185(4) 0.413(8) 0.0679(17) -0.063(3) -0.002(2) 0.071(5)
C25 0.152(9) 0.147(9) 0.021(3) 0.014(4) 0.001(4) 0.006(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
Rh1 C1 2.019(3) . ?
Rh1 C24 2.123(3) . ?
Rh1 C17 2.125(3) . ?
Rh1 C20 2.188(3) . ?
Rh1 C21 2.210(3) . ?
Rh1 Cl1 2.3940(8) . ?
N1 C1 1.344(4) . ?
N1 N2 1.382(4) . ?
N1 C11 1.437(4) . ?
N2 C2 1.310(4) . ?
N3 C1 1.380(4) . ?
N3 C2 1.391(4) . ?
N3 C6 1.415(4) . ?
C2 C3 1.427(5) . ?
C3 C4 1.345(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.445(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.409(4) . ?
C5 C10 1.414(5) . ?
C6 C7 1.396(4) . ?
C7 C8 1.391(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.395(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C16 1.387(5) . ?
C11 C12 1.392(4) . ?
C12 C13 1.393(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.392(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C24 1.414(4) . ?
C17 C18 1.523(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.542(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.510(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.385(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.516(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.532(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.518(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24 0.9500 . ?
Cl2 C25 1.791(11) . ?
Cl3 C25 1.722(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 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
C1 Rh1 C24 92.77(12) . . ?
C1 Rh1 C17 96.98(12) . . ?
C24 Rh1 C17 38.88(12) . . ?
C1 Rh1 C20 161.28(12) . . ?
C24 Rh1 C20 98.04(12) . . ?
C17 Rh1 C20 82.29(12) . . ?
C1 Rh1 C21 161.62(12) . . ?
C24 Rh1 C21 81.48(12) . . ?
C17 Rh1 C21 89.48(12) . . ?
C20 Rh1 C21 36.71(12) . . ?
C1 Rh1 Cl1 85.56(9) . . ?
C24 Rh1 Cl1 160.58(9) . . ?
C17 Rh1 Cl1 160.52(9) . . ?
C20 Rh1 Cl1 89.15(9) . . ?
C21 Rh1 Cl1 94.08(9) . . ?
C1 N1 N2 115.1(3) . . ?
C1 N1 C11 126.1(3) . . ?
N2 N1 C11 118.7(3) . . ?
C2 N2 N1 103.1(2) . . ?
C1 N3 C2 108.6(3) . . ?
C1 N3 C6 129.4(3) . . ?
C2 N3 C6 121.9(3) . . ?
N1 C1 N3 102.2(3) . . ?
N1 C1 Rh1 126.6(2) . . ?
N3 C1 Rh1 130.3(2) . . ?
N2 C2 N3 110.9(3) . . ?
N2 C2 C3 128.8(3) . . ?
N3 C2 C3 120.3(3) . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 121.2(3) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C10 118.0(3) . . ?
C6 C5 C4 120.6(3) . . ?
C10 C5 C4 121.4(3) . . ?
C7 C6 C5 121.2(3) . . ?
C7 C6 N3 122.0(3) . . ?
C5 C6 N3 116.8(3) . . ?
C8 C7 C6 118.9(3) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C7 C8 C9 120.8(3) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C10 C9 C8 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C5 120.9(3) . . ?
C9 C10 H10 119.6 . . ?
C5 C10 H10 119.6 . . ?
C16 C11 C12 121.9(3) . . ?
C16 C11 N1 118.6(3) . . ?
C12 C11 N1 119.5(3) . . ?
C11 C12 C13 118.3(3) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 120.6(3) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C16 119.9(3) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C11 C16 C15 118.9(3) . . ?
C11 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C24 C17 C18 124.4(3) . . ?
C24 C17 Rh1 70.49(18) . . ?
C18 C17 Rh1 112.7(2) . . ?
C24 C17 H17 117.8 . . ?
C18 C17 H17 117.8 . . ?
Rh1 C17 H17 86.9 . . ?
C17 C18 C19 113.0(3) . . ?
C17 C18 H18A 109.0 . . ?
C19 C18 H18A 109.0 . . ?
C17 C18 H18B 109.0 . . ?
C19 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C18 113.0(3) . . ?
C20 C19 H19A 109.0 . . ?
C18 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
C18 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C21 C20 C19 126.3(3) . . ?
C21 C20 Rh1 72.52(18) . . ?
C19 C20 Rh1 107.6(2) . . ?
C21 C20 H20 116.8 . . ?
C19 C20 H20 116.8 . . ?
Rh1 C20 H20 89.8 . . ?
C20 C21 C22 123.8(3) . . ?
C20 C21 Rh1 70.78(18) . . ?
C22 C21 Rh1 111.5(2) . . ?
C20 C21 H21 118.1 . . ?
C22 C21 H21 118.1 . . ?
Rh1 C21 H21 87.8 . . ?
C21 C22 C23 112.0(3) . . ?
C21 C22 H22A 109.2 . . ?
C23 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
C23 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C24 C23 C22 113.3(3) . . ?
C24 C23 H23A 108.9 . . ?
C22 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C22 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
C17 C24 C23 125.6(3) . . ?
C17 C24 Rh1 70.64(18) . . ?
C23 C24 Rh1 110.0(2) . . ?
C17 C24 H24 117.2 . . ?
C23 C24 H24 117.2 . . ?
Rh1 C24 H24 89.4 . . ?
Cl3 C25 Cl2 102.9(4) . . ?
Cl3 C25 H25A 111.2 . . ?
Cl2 C25 H25A 111.2 . . ?
Cl3 C25 H25B 111.2 . . ?
Cl2 C25 H25B 111.2 . . ?
H25A C25 H25B 109.1 . . ?

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
C1 N1 N2 C2 -0.6(3) . . . . ?
C11 N1 N2 C2 177.4(3) . . . . ?
N2 N1 C1 N3 0.9(3) . . . . ?
C11 N1 C1 N3 -177.0(3) . . . . ?
N2 N1 C1 Rh1 -169.7(2) . . . . ?
C11 N1 C1 Rh1 12.5(4) . . . . ?
C2 N3 C1 N1 -0.8(3) . . . . ?
C6 N3 C1 N1 175.5(3) . . . . ?
C2 N3 C1 Rh1 169.3(2) . . . . ?
C6 N3 C1 Rh1 -14.4(5) . . . . ?
C24 Rh1 C1 N1 -66.2(3) . . . . ?
C17 Rh1 C1 N1 -105.0(3) . . . . ?
C20 Rh1 C1 N1 168.4(3) . . . . ?
C21 Rh1 C1 N1 4.8(6) . . . . ?
Cl1 Rh1 C1 N1 94.4(3) . . . . ?
C24 Rh1 C1 N3 125.9(3) . . . . ?
C17 Rh1 C1 N3 87.1(3) . . . . ?
C20 Rh1 C1 N3 0.6(6) . . . . ?
C21 Rh1 C1 N3 -163.0(3) . . . . ?
Cl1 Rh1 C1 N3 -73.5(3) . . . . ?
N1 N2 C2 N3 0.0(3) . . . . ?
N1 N2 C2 C3 179.7(3) . . . . ?
C1 N3 C2 N2 0.5(4) . . . . ?
C6 N3 C2 N2 -176.1(3) . . . . ?
C1 N3 C2 C3 -179.2(3) . . . . ?
C6 N3 C2 C3 4.1(5) . . . . ?
N2 C2 C3 C4 177.5(3) . . . . ?
N3 C2 C3 C4 -2.8(5) . . . . ?
C2 C3 C4 C5 -0.9(5) . . . . ?
C3 C4 C5 C6 3.5(5) . . . . ?
C3 C4 C5 C10 -176.1(3) . . . . ?
C10 C5 C6 C7 -1.5(5) . . . . ?
C4 C5 C6 C7 178.9(3) . . . . ?
C10 C5 C6 N3 177.5(3) . . . . ?
C4 C5 C6 N3 -2.1(4) . . . . ?
C1 N3 C6 C7 1.5(5) . . . . ?
C2 N3 C6 C7 177.4(3) . . . . ?
C1 N3 C6 C5 -177.5(3) . . . . ?
C2 N3 C6 C5 -1.6(4) . . . . ?
C5 C6 C7 C8 2.1(5) . . . . ?
N3 C6 C7 C8 -176.9(3) . . . . ?
C6 C7 C8 C9 -1.0(5) . . . . ?
C7 C8 C9 C10 -0.7(6) . . . . ?
C8 C9 C10 C5 1.2(5) . . . . ?
C6 C5 C10 C9 -0.1(5) . . . . ?
C4 C5 C10 C9 179.4(3) . . . . ?
C1 N1 C11 C16 124.5(3) . . . . ?
N2 N1 C11 C16 -53.2(4) . . . . ?
C1 N1 C11 C12 -53.7(4) . . . . ?
N2 N1 C11 C12 128.5(3) . . . . ?
C16 C11 C12 C13 0.0(5) . . . . ?
N1 C11 C12 C13 178.2(3) . . . . ?
C11 C12 C13 C14 -0.1(5) . . . . ?
C12 C13 C14 C15 0.2(5) . . . . ?
C13 C14 C15 C16 0.0(5) . . . . ?
C12 C11 C16 C15 0.1(5) . . . . ?
N1 C11 C16 C15 -178.1(3) . . . . ?
C14 C15 C16 C11 -0.1(5) . . . . ?
C1 Rh1 C17 C24 85.7(2) . . . . ?
C20 Rh1 C17 C24 -113.1(2) . . . . ?
C21 Rh1 C17 C24 -77.0(2) . . . . ?
Cl1 Rh1 C17 C24 -177.8(2) . . . . ?
C1 Rh1 C17 C18 -154.1(2) . . . . ?
C24 Rh1 C17 C18 120.1(3) . . . . ?
C20 Rh1 C17 C18 7.0(2) . . . . ?
C21 Rh1 C17 C18 43.1(2) . . . . ?
Cl1 Rh1 C17 C18 -57.7(4) . . . . ?
C24 C17 C18 C19 92.6(4) . . . . ?
Rh1 C17 C18 C19 11.4(3) . . . . ?
C17 C18 C19 C20 -32.9(4) . . . . ?
C18 C19 C20 C21 -43.9(4) . . . . ?
C18 C19 C20 Rh1 37.0(3) . . . . ?
C1 Rh1 C20 C21 -171.4(3) . . . . ?
C24 Rh1 C20 C21 63.9(2) . . . . ?
C17 Rh1 C20 C21 99.6(2) . . . . ?
Cl1 Rh1 C20 C21 -97.98(18) . . . . ?
C1 Rh1 C20 C19 65.1(5) . . . . ?
C24 Rh1 C20 C19 -59.5(2) . . . . ?
C17 Rh1 C20 C19 -23.9(2) . . . . ?
C21 Rh1 C20 C19 -123.5(3) . . . . ?
Cl1 Rh1 C20 C19 138.6(2) . . . . ?
C19 C20 C21 C22 -4.1(5) . . . . ?
Rh1 C20 C21 C22 -103.5(3) . . . . ?
C19 C20 C21 Rh1 99.4(3) . . . . ?
C1 Rh1 C21 C20 171.3(3) . . . . ?
C24 Rh1 C21 C20 -115.9(2) . . . . ?
C17 Rh1 C21 C20 -77.7(2) . . . . ?
Cl1 Rh1 C21 C20 83.08(18) . . . . ?
C1 Rh1 C21 C22 -69.0(5) . . . . ?
C24 Rh1 C21 C22 3.8(2) . . . . ?
C17 Rh1 C21 C22 42.0(2) . . . . ?
C20 Rh1 C21 C22 119.8(3) . . . . ?
Cl1 Rh1 C21 C22 -157.2(2) . . . . ?
C20 C21 C22 C23 95.9(4) . . . . ?
Rh1 C21 C22 C23 15.2(3) . . . . ?
C21 C22 C23 C24 -35.0(4) . . . . ?
C18 C17 C24 C23 -3.4(5) . . . . ?
Rh1 C17 C24 C23 101.2(3) . . . . ?
C18 C17 C24 Rh1 -104.6(3) . . . . ?
C22 C23 C24 C17 -42.3(4) . . . . ?
C22 C23 C24 Rh1 37.7(3) . . . . ?
C1 Rh1 C24 C17 -97.69(19) . . . . ?
C20 Rh1 C24 C17 67.0(2) . . . . ?
C21 Rh1 C24 C17 99.9(2) . . . . ?
Cl1 Rh1 C24 C17 177.8(2) . . . . ?
C1 Rh1 C24 C23 140.4(2) . . . . ?
C17 Rh1 C24 C23 -121.9(3) . . . . ?
C20 Rh1 C24 C23 -54.9(2) . . . . ?
C21 Rh1 C24 C23 -22.0(2) . . . . ?
Cl1 Rh1 C24 C23 55.9(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.570
_refine_diff_density_min         -2.567
_refine_diff_density_rms         0.155

###END

# Attachment '19.cif'

#=========================================================================
# Data for compound 19 (local labelling ea08107x)
#=========================================================================

data_19
_database_code_depnum_ccdc_archive 'CCDC 727064'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H18 Cl N3 Pd'
_chemical_formula_sum            'C23 H18 Cl N3 Pd'
_chemical_formula_weight         478.25

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'
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                   9.5846(6)
_cell_length_b                   30.038(2)
_cell_length_c                   7.0204(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.420(3)
_cell_angle_gamma                90.00
_cell_volume                     1917.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2991
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      24.29

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7747
_exptl_absorpt_correction_T_max  0.8962
_exptl_absorpt_process_details   
;
SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
X-ray Solutions, Madison, Wisconsin, USA.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Bruker-Nonius X8kappa APEX II CCD area detector'
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15674
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         26.44
_reflns_number_total             3931
_reflns_number_gt                2577
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker (2006). APEX 2. Version 2.1.'
_computing_cell_refinement       'Bruker (2006). APEX 2. Version 2.1.'
_computing_data_reduction        'Bruker (2006). APEX 2. Version 2.1.'
_computing_structure_solution    'Bruker (2006). APEX 2. Version 2.1.'
_computing_structure_refinement  'XL, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL v. 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. 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^)+(0.0517P)^2^+4.0781P] 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         3931
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1274
_refine_ls_wR_factor_gt          0.1092
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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 0.77626(4) 0.063749(16) 0.90739(7) 0.02304(16) Uani 1 1 d . . .
Cl1 Cl 0.88361(15) 0.05271(5) 0.6500(2) 0.0293(4) Uani 1 1 d . . .
N1 N 0.8049(5) 0.16913(16) 0.8828(7) 0.0196(11) Uani 1 1 d . . .
N2 N 0.5917(5) 0.14382(17) 0.7433(7) 0.0222(11) Uani 1 1 d . . .
N3 N 0.5756(5) 0.18921(17) 0.7208(7) 0.0213(11) Uani 1 1 d . . .
C1 C 0.7294(6) 0.1291(2) 0.8448(8) 0.0213(13) Uani 1 1 d . . .
C2 C 0.7086(6) 0.2035(2) 0.8094(8) 0.0201(13) Uani 1 1 d . . .
C3 C 0.7554(6) 0.2490(2) 0.8377(8) 0.0235(14) Uani 1 1 d . . .
C4 C 0.9026(6) 0.2582(2) 0.9513(8) 0.0229(13) Uani 1 1 d . . .
C5 C 0.9440(7) 0.3032(2) 0.9851(9) 0.0270(14) Uani 1 1 d . . .
H5 H 1.0426 0.3105 1.0596 0.032 Uiso 1 1 calc R . .
C6 C 0.8438(7) 0.3365(2) 0.9120(10) 0.0324(15) Uani 1 1 d . . .
H6 H 0.8737 0.3667 0.9379 0.039 Uiso 1 1 calc R . .
C7 C 0.7000(7) 0.3270(2) 0.8011(9) 0.0289(15) Uani 1 1 d . . .
H7 H 0.6322 0.3505 0.7505 0.035 Uiso 1 1 calc R . .
C8 C 0.6554(6) 0.2838(2) 0.7641(9) 0.0256(14) Uani 1 1 d . . .
H8 H 0.5563 0.2773 0.6884 0.031 Uiso 1 1 calc R . .
C9 C 1.0039(6) 0.2206(2) 1.0245(8) 0.0222(13) Uani 1 1 d . . .
C10 C 0.9556(6) 0.1765(2) 0.9903(8) 0.0203(13) Uani 1 1 d . . .
C11 C 1.0490(6) 0.1409(2) 1.0595(9) 0.0280(15) Uani 1 1 d . . .
H11 H 1.0148 0.1113 1.0298 0.034 Uiso 1 1 calc R . .
C12 C 1.1937(6) 0.1493(2) 1.1731(9) 0.0318(16) Uani 1 1 d . . .
H12 H 1.2584 0.1250 1.2239 0.038 Uiso 1 1 calc R . .
C13 C 1.2447(6) 0.1921(2) 1.2133(9) 0.0293(15) Uani 1 1 d . . .
H13 H 1.3438 0.1974 1.2924 0.035 Uiso 1 1 calc R . .
C14 C 1.1528(6) 0.2269(2) 1.1393(9) 0.0279(15) Uani 1 1 d . . .
H14 H 1.1899 0.2564 1.1656 0.034 Uiso 1 1 calc R . .
C15 C 0.4651(5) 0.11612(19) 0.6719(8) 0.0191(12) Uani 1 1 d . . .
C16 C 0.3380(6) 0.1278(2) 0.7167(10) 0.0293(15) Uani 1 1 d . . .
H16 H 0.3349 0.1543 0.7890 0.035 Uiso 1 1 calc R . .
C17 C 0.2171(6) 0.1002(2) 0.6541(10) 0.0308(16) Uani 1 1 d . . .
H17 H 0.1298 0.1079 0.6830 0.037 Uiso 1 1 calc R . .
C18 C 0.2217(6) 0.0615(2) 0.5498(9) 0.0324(16) Uani 1 1 d . . .
H18 H 0.1376 0.0428 0.5065 0.039 Uiso 1 1 calc R . .
C19 C 0.3506(6) 0.0499(2) 0.5079(9) 0.0300(15) Uani 1 1 d . . .
H19 H 0.3545 0.0229 0.4393 0.036 Uiso 1 1 calc R . .
C20 C 0.4720(6) 0.0776(2) 0.5662(9) 0.0247(14) Uani 1 1 d . . .
H20 H 0.5586 0.0703 0.5345 0.030 Uiso 1 1 calc R . .
C21 C 0.7799(8) -0.0056(2) 0.9961(11) 0.0420(18) Uani 1 1 d . . .
H21A H 0.7101 -0.0015 0.8668 0.050 Uiso 1 1 calc R . .
H21B H 0.8532 -0.0280 1.0166 0.050 Uiso 1 1 calc R . .
C22 C 0.7750(11) 0.0198(3) 1.1468(14) 0.061(2) Uani 1 1 d . . .
H22 H 0.8456 0.0152 1.2752 0.074 Uiso 1 1 calc R . .
C23 C 0.6676(7) 0.0537(2) 1.1233(11) 0.0408(19) Uani 1 1 d . . .
H23A H 0.5963 0.0586 0.9958 0.049 Uiso 1 1 calc R . .
H23B H 0.6670 0.0714 1.2350 0.049 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 0.0230(2) 0.0266(3) 0.0201(2) 0.0016(2) 0.00769(16) -0.0019(2)
Cl1 0.0296(7) 0.0330(10) 0.0299(9) 0.0015(7) 0.0158(6) 0.0012(6)
N1 0.022(2) 0.026(3) 0.015(3) 0.003(2) 0.0119(19) -0.0011(19)
N2 0.020(2) 0.024(3) 0.024(3) 0.000(2) 0.010(2) -0.003(2)
N3 0.026(2) 0.024(3) 0.017(3) 0.001(2) 0.011(2) -0.001(2)
C1 0.020(3) 0.035(4) 0.012(3) -0.003(3) 0.009(2) -0.006(2)
C2 0.025(3) 0.025(4) 0.012(3) 0.000(3) 0.009(2) -0.002(2)
C3 0.028(3) 0.033(4) 0.013(3) 0.001(3) 0.013(3) -0.001(3)
C4 0.033(3) 0.031(4) 0.010(3) -0.001(3) 0.014(2) -0.006(3)
C5 0.037(3) 0.030(4) 0.018(3) -0.007(3) 0.014(3) -0.010(3)
C6 0.057(4) 0.023(4) 0.025(4) -0.003(3) 0.024(3) -0.006(3)
C7 0.043(4) 0.028(4) 0.024(4) 0.001(3) 0.023(3) 0.001(3)
C8 0.034(3) 0.027(4) 0.022(3) 0.000(3) 0.017(3) -0.001(3)
C9 0.027(3) 0.034(4) 0.011(3) -0.001(3) 0.013(2) -0.010(3)
C10 0.021(3) 0.035(4) 0.009(3) 0.000(3) 0.011(2) -0.005(2)
C11 0.024(3) 0.034(4) 0.026(4) 0.003(3) 0.007(3) -0.006(3)
C12 0.023(3) 0.049(5) 0.023(3) 0.003(3) 0.007(3) -0.003(3)
C13 0.024(3) 0.045(4) 0.021(3) 0.004(3) 0.010(2) -0.008(3)
C14 0.031(3) 0.038(4) 0.017(3) -0.007(3) 0.011(3) -0.013(3)
C15 0.019(2) 0.025(3) 0.013(3) 0.005(2) 0.005(2) -0.001(2)
C16 0.030(3) 0.030(4) 0.029(4) 0.002(3) 0.011(3) 0.000(3)
C17 0.026(3) 0.036(4) 0.034(4) 0.010(3) 0.014(3) 0.003(3)
C18 0.025(3) 0.031(4) 0.038(4) 0.007(3) 0.006(3) -0.004(3)
C19 0.033(3) 0.025(4) 0.029(4) -0.004(3) 0.005(3) -0.004(3)
C20 0.028(3) 0.029(4) 0.019(3) 0.002(3) 0.009(2) -0.001(2)
C21 0.069(5) 0.032(4) 0.025(4) 0.014(3) 0.015(3) 0.011(3)
C22 0.096(7) 0.048(6) 0.050(6) 0.016(4) 0.037(5) -0.001(5)
C23 0.046(4) 0.055(5) 0.030(4) 0.020(3) 0.026(3) 0.002(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.031(6) . ?
Pd1 C23 2.115(6) . ?
Pd1 C22 2.141(8) . ?
Pd1 C21 2.172(7) . ?
Pd1 Cl1 2.3680(16) . ?
N1 C2 1.372(7) . ?
N1 C1 1.386(7) . ?
N1 C10 1.420(6) . ?
N2 C1 1.360(7) . ?
N2 N3 1.376(6) . ?
N2 C15 1.426(7) . ?
N3 C2 1.303(7) . ?
C2 C3 1.432(8) . ?
C3 C8 1.403(8) . ?
C3 C4 1.411(7) . ?
C4 C5 1.406(8) . ?
C4 C9 1.473(8) . ?
C5 C6 1.370(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.382(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.364(9) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.397(8) . ?
C9 C14 1.413(7) . ?
C10 C11 1.380(8) . ?
C11 C12 1.386(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.374(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.360(9) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.388(8) . ?
C15 C16 1.395(8) . ?
C16 C17 1.378(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.401(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(8) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.317(11) . ?
C21 H21A 0.9500 . ?
C21 H21B 0.9500 . ?
C22 C23 1.421(11) . ?
C22 H22 0.9500 . ?
C23 H23A 0.9500 . ?
C23 H23B 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 C23 99.7(3) . . ?
C1 Pd1 C22 135.3(3) . . ?
C23 Pd1 C22 39.0(3) . . ?
C1 Pd1 C21 166.4(2) . . ?
C23 Pd1 C21 67.9(3) . . ?
C22 Pd1 C21 35.5(3) . . ?
C1 Pd1 Cl1 95.17(16) . . ?
C23 Pd1 Cl1 163.3(2) . . ?
C22 Pd1 Cl1 128.6(2) . . ?
C21 Pd1 Cl1 96.5(2) . . ?
C2 N1 C1 109.4(4) . . ?
C2 N1 C10 122.2(5) . . ?
C1 N1 C10 128.3(5) . . ?
C1 N2 N3 116.0(4) . . ?
C1 N2 C15 124.9(5) . . ?
N3 N2 C15 119.0(4) . . ?
C2 N3 N2 102.4(4) . . ?
N2 C1 N1 100.4(5) . . ?
N2 C1 Pd1 122.6(4) . . ?
N1 C1 Pd1 137.0(4) . . ?
N3 C2 N1 111.8(5) . . ?
N3 C2 C3 126.7(5) . . ?
N1 C2 C3 121.5(5) . . ?
C8 C3 C4 120.4(6) . . ?
C8 C3 C2 120.8(5) . . ?
C4 C3 C2 118.6(5) . . ?
C5 C4 C3 117.6(6) . . ?
C5 C4 C9 123.9(5) . . ?
C3 C4 C9 118.5(5) . . ?
C6 C5 C4 120.8(6) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 121.0(6) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 120.1(6) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C3 120.1(6) . . ?
C7 C8 H8 119.9 . . ?
C3 C8 H8 119.9 . . ?
C10 C9 C14 116.5(6) . . ?
C10 C9 C4 121.4(5) . . ?
C14 C9 C4 122.1(5) . . ?
C11 C10 C9 122.0(5) . . ?
C11 C10 N1 120.2(5) . . ?
C9 C10 N1 117.7(5) . . ?
C10 C11 C12 118.8(6) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 120.9(6) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C14 C13 C12 119.8(6) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C9 121.9(6) . . ?
C13 C14 H14 119.0 . . ?
C9 C14 H14 119.0 . . ?
C20 C15 C16 121.5(5) . . ?
C20 C15 N2 119.7(5) . . ?
C16 C15 N2 118.8(5) . . ?
C17 C16 C15 118.9(6) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C16 C17 C18 120.7(6) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C17 C18 C19 119.9(6) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 120.2(6) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C15 118.8(5) . . ?
C19 C20 H20 120.6 . . ?
C15 C20 H20 120.6 . . ?
C22 C21 Pd1 70.9(5) . . ?
C22 C21 H21A 120.0 . . ?
Pd1 C21 H21A 70.1 . . ?
C22 C21 H21B 120.0 . . ?
Pd1 C21 H21B 131.9 . . ?
H21A C21 H21B 120.0 . . ?
C21 C22 C23 122.0(8) . . ?
C21 C22 Pd1 73.5(5) . . ?
C23 C22 Pd1 69.5(4) . . ?
C21 C22 H22 119.0 . . ?
C23 C22 H22 119.0 . . ?
Pd1 C22 H22 130.8 . . ?
C22 C23 Pd1 71.5(4) . . ?
C22 C23 H23A 120.0 . . ?
Pd1 C23 H23A 70.9 . . ?
C22 C23 H23B 120.0 . . ?
Pd1 C23 H23B 130.1 . . ?
H23A C23 H23B 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
C1 N2 N3 C2 0.8(6) . . . . ?
C15 N2 N3 C2 177.0(5) . . . . ?
N3 N2 C1 N1 -1.7(6) . . . . ?
C15 N2 C1 N1 -177.7(5) . . . . ?
N3 N2 C1 Pd1 176.9(4) . . . . ?
C15 N2 C1 Pd1 1.0(7) . . . . ?
C2 N1 C1 N2 1.9(6) . . . . ?
C10 N1 C1 N2 178.2(5) . . . . ?
C2 N1 C1 Pd1 -176.4(5) . . . . ?
C10 N1 C1 Pd1 -0.1(9) . . . . ?
C23 Pd1 C1 N2 -70.0(5) . . . . ?
C22 Pd1 C1 N2 -88.4(6) . . . . ?
C21 Pd1 C1 N2 -46.3(13) . . . . ?
Cl1 Pd1 C1 N2 102.4(4) . . . . ?
C23 Pd1 C1 N1 108.1(6) . . . . ?
C22 Pd1 C1 N1 89.7(7) . . . . ?
C21 Pd1 C1 N1 131.8(10) . . . . ?
Cl1 Pd1 C1 N1 -79.5(6) . . . . ?
N2 N3 C2 N1 0.5(6) . . . . ?
N2 N3 C2 C3 -177.5(5) . . . . ?
C1 N1 C2 N3 -1.7(6) . . . . ?
C10 N1 C2 N3 -178.2(4) . . . . ?
C1 N1 C2 C3 176.5(5) . . . . ?
C10 N1 C2 C3 -0.1(8) . . . . ?
N3 C2 C3 C8 -1.2(9) . . . . ?
N1 C2 C3 C8 -179.1(5) . . . . ?
N3 C2 C3 C4 175.1(5) . . . . ?
N1 C2 C3 C4 -2.8(8) . . . . ?
C8 C3 C4 C5 -0.6(8) . . . . ?
C2 C3 C4 C5 -177.0(5) . . . . ?
C8 C3 C4 C9 -179.7(5) . . . . ?
C2 C3 C4 C9 3.9(8) . . . . ?
C3 C4 C5 C6 0.8(8) . . . . ?
C9 C4 C5 C6 179.9(6) . . . . ?
C4 C5 C6 C7 -0.8(9) . . . . ?
C5 C6 C7 C8 0.5(10) . . . . ?
C6 C7 C8 C3 -0.3(9) . . . . ?
C4 C3 C8 C7 0.4(9) . . . . ?
C2 C3 C8 C7 176.7(5) . . . . ?
C5 C4 C9 C10 178.5(5) . . . . ?
C3 C4 C9 C10 -2.5(8) . . . . ?
C5 C4 C9 C14 1.0(9) . . . . ?
C3 C4 C9 C14 -180.0(5) . . . . ?
C14 C9 C10 C11 -1.8(8) . . . . ?
C4 C9 C10 C11 -179.5(5) . . . . ?
C14 C9 C10 N1 177.3(5) . . . . ?
C4 C9 C10 N1 -0.3(8) . . . . ?
C2 N1 C10 C11 -179.2(5) . . . . ?
C1 N1 C10 C11 4.9(8) . . . . ?
C2 N1 C10 C9 1.6(7) . . . . ?
C1 N1 C10 C9 -174.3(5) . . . . ?
C9 C10 C11 C12 2.6(9) . . . . ?
N1 C10 C11 C12 -176.6(5) . . . . ?
C10 C11 C12 C13 -1.3(9) . . . . ?
C11 C12 C13 C14 -0.6(9) . . . . ?
C12 C13 C14 C9 1.3(9) . . . . ?
C10 C9 C14 C13 -0.1(8) . . . . ?
C4 C9 C14 C13 177.4(5) . . . . ?
C1 N2 C15 C20 -48.0(8) . . . . ?
N3 N2 C15 C20 136.1(5) . . . . ?
C1 N2 C15 C16 129.7(6) . . . . ?
N3 N2 C15 C16 -46.1(7) . . . . ?
C20 C15 C16 C17 0.0(9) . . . . ?
N2 C15 C16 C17 -177.7(5) . . . . ?
C15 C16 C17 C18 0.4(9) . . . . ?
C16 C17 C18 C19 0.4(9) . . . . ?
C17 C18 C19 C20 -1.6(9) . . . . ?
C18 C19 C20 C15 2.0(9) . . . . ?
C16 C15 C20 C19 -1.2(9) . . . . ?
N2 C15 C20 C19 176.4(5) . . . . ?
C1 Pd1 C21 C22 -54.3(13) . . . . ?
C23 Pd1 C21 C22 -29.0(5) . . . . ?
Cl1 Pd1 C21 C22 157.1(5) . . . . ?
Pd1 C21 C22 C23 52.0(7) . . . . ?
C1 Pd1 C22 C21 164.2(4) . . . . ?
C23 Pd1 C22 C21 134.5(8) . . . . ?
Cl1 Pd1 C22 C21 -29.6(7) . . . . ?
C1 Pd1 C22 C23 29.7(7) . . . . ?
C21 Pd1 C22 C23 -134.5(8) . . . . ?
Cl1 Pd1 C22 C23 -164.1(4) . . . . ?
C21 C22 C23 Pd1 -53.8(7) . . . . ?
C1 Pd1 C23 C22 -159.3(5) . . . . ?
C21 Pd1 C23 C22 26.6(5) . . . . ?
Cl1 Pd1 C23 C22 48.1(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.44
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.460
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.140

###END