# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012


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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_5ppchuym
_database_code_depnum_ccdc_archive 'CCDC 873200'
#TrackingRef '5ppchuym.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C18 H16 N5), 3(Cl4 Pt), 4(H2 O)'
_chemical_formula_sum            'C36 H40 Cl12 N10 O4 Pt3'
_chemical_formula_weight         1687.45

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.4937(13)
_cell_length_b                   11.609(2)
_cell_length_c                   14.781(3)
_cell_angle_alpha                102.927(3)
_cell_angle_beta                 102.710(3)
_cell_angle_gamma                93.364(3)
_cell_volume                     1214.6(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4293
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      27.59

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             796
_exptl_absorpt_coefficient_mu    9.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_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  '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            11670
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4257
_reflns_number_gt                3746
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_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^)+(0.0330P)^2^+16.4494P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4257
_refine_ls_number_parameters     316
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1154
_refine_ls_wR_factor_gt          0.1103
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.142
_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
Pt1 Pt 0.99096(6) 0.77987(4) 0.70984(3) 0.01526(14) Uani 1 1 d . . .
Pt2 Pt 0.0000 0.5000 0.0000 0.0371(2) Uani 1 2 d S . .
Cl1 Cl 1.3002(4) 0.7602(3) 0.7549(2) 0.0243(7) Uani 1 1 d . . .
Cl2 Cl 1.0440(4) 0.9595(2) 0.8228(2) 0.0240(6) Uani 1 1 d . . .
Cl3 Cl 0.6821(4) 0.7989(2) 0.6634(2) 0.0233(6) Uani 1 1 d . . .
Cl4 Cl 0.9463(4) 0.6009(3) 0.5982(2) 0.0264(7) Uani 1 1 d . . .
Cl5 Cl 0.0400(5) 0.6997(3) 0.0787(2) 0.0411(9) Uani 1 1 d . . .
Cl6 Cl 0.2988(6) 0.5073(3) -0.0108(3) 0.0568(11) Uani 1 1 d . . .
N1 N 0.6422(13) 1.0025(8) 0.3332(7) 0.022(2) Uani 1 1 d D . .
H1' H 0.672(17) 1.064(7) 0.317(9) 0.033 Uiso 1 1 d D . .
N2 N 0.6724(12) 0.8800(8) 0.4289(7) 0.021(2) Uani 1 1 d . . .
N3 N 0.9462(14) 1.2665(9) 0.6632(8) 0.027(2) Uani 1 1 d D . .
H3' H 1.000(16) 1.324(8) 0.708(7) 0.041 Uiso 1 1 d D . .
N4 N 0.3619(15) 0.8554(10) -0.0179(7) 0.029(2) Uani 1 1 d D . .
H4' H 0.319(18) 0.853(13) -0.076(3) 0.043 Uiso 1 1 d D . .
N5 N 0.4343(14) 0.4508(8) 0.2982(8) 0.026(2) Uani 1 1 d D . .
H5' H 0.397(17) 0.379(3) 0.292(10) 0.039 Uiso 1 1 d D . .
C1 C 0.6974(15) 0.9905(10) 0.4238(8) 0.018(2) Uani 1 1 d . . .
C2 C 0.5773(15) 0.8918(10) 0.2753(8) 0.020(3) Uani 1 1 d . . .
C3 C 0.5956(16) 0.8169(10) 0.3382(9) 0.023(3) Uani 1 1 d . . .
C4 C 0.7820(16) 1.0888(10) 0.5074(8) 0.022(3) Uani 1 1 d . . .
C5 C 0.8095(16) 1.2065(11) 0.4996(9) 0.026(3) Uani 1 1 d . . .
H5 H 0.7704 1.2256 0.4396 0.031 Uiso 1 1 calc R . .
C6 C 0.8921(17) 1.2921(11) 0.5782(10) 0.030(3) Uani 1 1 d . . .
H6 H 0.9122 1.3718 0.5732 0.036 Uiso 1 1 calc R . .
C7 C 0.9196(18) 1.1554(11) 0.6742(10) 0.033(3) Uani 1 1 d . . .
H7 H 0.9569 1.1403 0.7358 0.039 Uiso 1 1 calc R . .
C8 C 0.8400(16) 1.0653(11) 0.5981(9) 0.027(3) Uani 1 1 d . . .
H8 H 0.8233 0.9866 0.6057 0.032 Uiso 1 1 calc R . .
C9 C 0.5054(15) 0.8777(10) 0.1730(8) 0.020(3) Uani 1 1 d . . .
C10 C 0.3887(15) 0.9579(11) 0.1411(9) 0.023(3) Uani 1 1 d . . .
H10 H 0.3598 1.0218 0.1861 0.027 Uiso 1 1 calc R . .
C11 C 0.3157(16) 0.9448(11) 0.0448(9) 0.028(3) Uani 1 1 d . . .
H11 H 0.2341 0.9979 0.0231 0.033 Uiso 1 1 calc R . .
C12 C 0.4748(17) 0.7770(11) 0.0084(10) 0.032(3) Uani 1 1 d . . .
H12 H 0.5033 0.7154 -0.0388 0.038 Uiso 1 1 calc R . .
C13 C 0.5500(17) 0.7864(10) 0.1047(9) 0.026(3) Uani 1 1 d . . .
H13 H 0.6308 0.7317 0.1241 0.031 Uiso 1 1 calc R . .
C14 C 0.5359(15) 0.6876(10) 0.3215(8) 0.021(3) Uani 1 1 d . . .
C15 C 0.4142(17) 0.6221(11) 0.2378(9) 0.027(3) Uani 1 1 d . . .
H15 H 0.3662 0.6591 0.1879 0.033 Uiso 1 1 calc R . .
C16 C 0.3646(17) 0.5042(11) 0.2283(9) 0.027(3) Uani 1 1 d . . .
H16 H 0.2802 0.4594 0.1718 0.032 Uiso 1 1 calc R . .
C17 C 0.5514(18) 0.5108(11) 0.3787(10) 0.031(3) Uani 1 1 d . . .
H17 H 0.5987 0.4710 0.4269 0.037 Uiso 1 1 calc R . .
C18 C 0.6042(16) 0.6302(10) 0.3924(8) 0.022(3) Uani 1 1 d . . .
H18 H 0.6871 0.6730 0.4501 0.027 Uiso 1 1 calc R . .
O31 O 0.7753(13) 0.7693(9) 0.8996(7) 0.037(2) Uani 1 1 d D . .
H31A H 0.852(16) 0.760(14) 0.947(7) 0.055 Uiso 1 1 d D . .
H31B H 0.826(18) 0.802(13) 0.865(9) 0.055 Uiso 1 1 d D . .
O32 O 0.1392(16) 0.4709(8) 0.77215(19) 0.050(3) Uani 1 1 d D . .
H32A H 0.1482 0.4995 0.8307 0.074 Uiso 1 1 d D . .
H32B H 0.13(2) 0.515(12) 0.734(9) 0.074 Uiso 1 1 d 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
Pt1 0.0182(2) 0.0133(2) 0.0154(3) 0.00312(17) 0.00672(17) 0.00210(16)
Pt2 0.0618(5) 0.0221(4) 0.0218(4) 0.0047(3) -0.0010(4) 0.0045(4)
Cl1 0.0250(15) 0.0254(16) 0.0227(16) 0.0036(13) 0.0076(12) 0.0060(12)
Cl2 0.0295(15) 0.0190(15) 0.0214(16) 0.0015(12) 0.0050(12) 0.0043(12)
Cl3 0.0231(14) 0.0210(15) 0.0278(17) 0.0086(13) 0.0075(12) 0.0034(12)
Cl4 0.0354(17) 0.0191(15) 0.0224(16) 0.0021(13) 0.0051(13) 0.0049(12)
Cl5 0.063(2) 0.0234(17) 0.0295(19) 0.0022(15) -0.0008(17) 0.0040(16)
Cl6 0.081(3) 0.038(2) 0.042(2) -0.0004(18) 0.006(2) 0.008(2)
N1 0.027(5) 0.017(5) 0.024(6) 0.012(5) 0.003(4) 0.006(4)
N2 0.024(5) 0.021(5) 0.018(5) 0.002(4) 0.004(4) 0.006(4)
N3 0.032(6) 0.023(6) 0.025(6) 0.005(5) 0.003(5) 0.002(5)
N4 0.038(6) 0.033(6) 0.020(6) 0.009(5) 0.015(5) 0.003(5)
N5 0.034(6) 0.013(5) 0.036(7) 0.005(5) 0.021(5) 0.005(5)
C1 0.022(6) 0.021(6) 0.011(6) 0.002(5) 0.007(5) 0.006(5)
C2 0.026(6) 0.019(6) 0.015(6) 0.007(5) 0.002(5) 0.002(5)
C3 0.027(6) 0.022(6) 0.025(7) 0.009(5) 0.013(5) 0.010(5)
C4 0.025(6) 0.023(6) 0.022(7) 0.011(5) 0.005(5) 0.007(5)
C5 0.032(7) 0.026(7) 0.021(7) 0.007(6) 0.007(5) 0.006(5)
C6 0.036(7) 0.019(7) 0.040(8) 0.011(6) 0.016(6) 0.008(6)
C7 0.045(8) 0.020(7) 0.034(8) 0.012(6) 0.005(6) 0.002(6)
C8 0.033(7) 0.021(7) 0.026(7) 0.009(6) 0.003(6) 0.001(5)
C9 0.022(6) 0.016(6) 0.027(7) 0.009(5) 0.012(5) -0.001(5)
C10 0.021(6) 0.025(7) 0.023(7) 0.006(5) 0.006(5) 0.005(5)
C11 0.028(7) 0.024(7) 0.035(8) 0.009(6) 0.014(6) 0.004(5)
C12 0.031(7) 0.022(7) 0.038(8) -0.006(6) 0.017(6) -0.007(6)
C13 0.033(7) 0.020(6) 0.025(7) 0.007(5) 0.008(6) 0.004(5)
C14 0.026(6) 0.024(6) 0.019(7) 0.008(5) 0.016(5) 0.008(5)
C15 0.035(7) 0.022(7) 0.024(7) 0.006(6) 0.006(6) -0.003(5)
C16 0.035(7) 0.027(7) 0.025(7) 0.012(6) 0.012(6) 0.009(6)
C17 0.039(8) 0.025(7) 0.029(8) 0.009(6) 0.008(6) 0.008(6)
C18 0.029(6) 0.024(7) 0.018(7) 0.010(5) 0.007(5) 0.007(5)
O31 0.040(6) 0.042(6) 0.033(6) 0.014(5) 0.013(4) 0.005(5)
O32 0.075(8) 0.034(6) 0.037(6) 0.006(5) 0.011(6) 0.004(5)

_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
Pt1 Cl4 2.301(3) . ?
Pt1 Cl3 2.304(3) . ?
Pt1 Cl1 2.306(3) . ?
Pt1 Cl2 2.312(3) . ?
Pt2 Cl6 2.278(5) . ?
Pt2 Cl6 2.278(5) 2_565 ?
Pt2 Cl5 2.318(3) 2_565 ?
Pt2 Cl5 2.318(3) . ?
N1 C1 1.353(14) . ?
N1 C2 1.368(15) . ?
N2 C1 1.307(14) . ?
N2 C3 1.355(15) . ?
N3 C6 1.337(16) . ?
N3 C7 1.344(15) . ?
N4 C12 1.340(17) . ?
N4 C11 1.345(16) . ?
N5 C17 1.329(16) . ?
N5 C16 1.346(16) . ?
C1 C4 1.473(16) . ?
C2 C3 1.400(16) . ?
C2 C9 1.457(16) . ?
C3 C14 1.490(16) . ?
C4 C5 1.405(16) . ?
C4 C8 1.408(16) . ?
C5 C6 1.348(17) . ?
C7 C8 1.349(17) . ?
C9 C13 1.402(16) . ?
C9 C10 1.402(16) . ?
C10 C11 1.377(17) . ?
C12 C13 1.389(18) . ?
C14 C18 1.385(16) . ?
C14 C15 1.394(16) . ?
C15 C16 1.364(17) . ?
C17 C18 1.376(17) . ?

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
Cl4 Pt1 Cl3 89.55(10) . . ?
Cl4 Pt1 Cl1 90.07(10) . . ?
Cl3 Pt1 Cl1 179.48(11) . . ?
Cl4 Pt1 Cl2 178.52(11) . . ?
Cl3 Pt1 Cl2 91.92(10) . . ?
Cl1 Pt1 Cl2 88.46(10) . . ?
Cl6 Pt2 Cl6 180.0(2) . 2_565 ?
Cl6 Pt2 Cl5 88.62(13) . 2_565 ?
Cl6 Pt2 Cl5 91.38(13) 2_565 2_565 ?
Cl6 Pt2 Cl5 91.38(13) . . ?
Cl6 Pt2 Cl5 88.62(13) 2_565 . ?
Cl5 Pt2 Cl5 180.0(2) 2_565 . ?
C1 N1 C2 107.7(9) . . ?
C1 N2 C3 105.6(10) . . ?
C6 N3 C7 121.8(11) . . ?
C12 N4 C11 123.4(11) . . ?
C17 N5 C16 121.5(11) . . ?
N2 C1 N1 112.1(10) . . ?
N2 C1 C4 123.2(10) . . ?
N1 C1 C4 124.7(10) . . ?
N1 C2 C3 104.1(10) . . ?
N1 C2 C9 119.9(10) . . ?
C3 C2 C9 136.0(11) . . ?
N2 C3 C2 110.4(10) . . ?
N2 C3 C14 118.6(10) . . ?
C2 C3 C14 130.9(11) . . ?
C5 C4 C8 118.2(11) . . ?
C5 C4 C1 122.0(10) . . ?
C8 C4 C1 119.8(10) . . ?
C6 C5 C4 119.2(12) . . ?
N3 C6 C5 120.9(12) . . ?
N3 C7 C8 120.3(12) . . ?
C7 C8 C4 119.5(12) . . ?
C13 C9 C10 118.4(11) . . ?
C13 C9 C2 122.1(11) . . ?
C10 C9 C2 119.5(10) . . ?
C11 C10 C9 120.5(11) . . ?
N4 C11 C10 118.8(12) . . ?
N4 C12 C13 119.7(12) . . ?
C12 C13 C9 119.2(11) . . ?
C18 C14 C15 118.6(11) . . ?
C18 C14 C3 118.5(11) . . ?
C15 C14 C3 122.9(11) . . ?
C16 C15 C14 119.4(12) . . ?
N5 C16 C15 120.6(12) . . ?
N5 C17 C18 120.3(12) . . ?
C17 C18 C14 119.7(11) . . ?

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
C3 N2 C1 N1 -0.8(13) . . . . ?
C3 N2 C1 C4 -178.8(10) . . . . ?
C2 N1 C1 N2 -0.2(13) . . . . ?
C2 N1 C1 C4 177.7(10) . . . . ?
C1 N1 C2 C3 1.1(12) . . . . ?
C1 N1 C2 C9 179.1(10) . . . . ?
C1 N2 C3 C2 1.5(13) . . . . ?
C1 N2 C3 C14 -175.1(10) . . . . ?
N1 C2 C3 N2 -1.6(13) . . . . ?
C9 C2 C3 N2 -179.1(12) . . . . ?
N1 C2 C3 C14 174.4(11) . . . . ?
C9 C2 C3 C14 -3(2) . . . . ?
N2 C1 C4 C5 179.1(11) . . . . ?
N1 C1 C4 C5 1.3(17) . . . . ?
N2 C1 C4 C8 -0.1(17) . . . . ?
N1 C1 C4 C8 -177.8(11) . . . . ?
C8 C4 C5 C6 0.9(17) . . . . ?
C1 C4 C5 C6 -178.3(11) . . . . ?
C7 N3 C6 C5 -0.6(19) . . . . ?
C4 C5 C6 N3 -0.6(18) . . . . ?
C6 N3 C7 C8 1.5(19) . . . . ?
N3 C7 C8 C4 -1.1(19) . . . . ?
C5 C4 C8 C7 0.0(18) . . . . ?
C1 C4 C8 C7 179.2(11) . . . . ?
N1 C2 C9 C13 136.0(12) . . . . ?
C3 C2 C9 C13 -47(2) . . . . ?
N1 C2 C9 C10 -43.6(15) . . . . ?
C3 C2 C9 C10 133.6(14) . . . . ?
C13 C9 C10 C11 1.9(17) . . . . ?
C2 C9 C10 C11 -178.5(10) . . . . ?
C12 N4 C11 C10 0.6(18) . . . . ?
C9 C10 C11 N4 -1.6(17) . . . . ?
C11 N4 C12 C13 0.0(18) . . . . ?
N4 C12 C13 C9 0.3(18) . . . . ?
C10 C9 C13 C12 -1.3(17) . . . . ?
C2 C9 C13 C12 179.2(11) . . . . ?
N2 C3 C14 C18 -17.3(16) . . . . ?
C2 C3 C14 C18 167.0(12) . . . . ?
N2 C3 C14 C15 162.6(11) . . . . ?
C2 C3 C14 C15 -13.2(19) . . . . ?
C18 C14 C15 C16 0.6(17) . . . . ?
C3 C14 C15 C16 -179.3(11) . . . . ?
C17 N5 C16 C15 0.7(18) . . . . ?
C14 C15 C16 N5 -1.0(18) . . . . ?
C16 N5 C17 C18 0.1(18) . . . . ?
N5 C17 C18 C14 -0.5(18) . . . . ?
C15 C14 C18 C17 0.2(17) . . . . ?
C3 C14 C18 C17 -180.0(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.394
_refine_diff_density_min         -3.935
_refine_diff_density_rms         0.241


data_j5crachm
_database_code_depnum_ccdc_archive 'CCDC 873201'
#TrackingRef 'j5crachm.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H16 N5, Cl4 Cu, Cl'
_chemical_formula_sum            'C18 H16 Cl5 Cu N5'
_chemical_formula_weight         543.15

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'
Cu Cu 0.3201 1.2651 '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

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                   6.9399(8)
_cell_length_b                   14.5758(17)
_cell_length_c                   21.126(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.407(2)
_cell_angle_gamma                90.00
_cell_volume                     2135.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      28.24

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            'light orange'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_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  '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            20227
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3766
_reflns_number_gt                3600
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_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^)+(0.0304P)^2^+3.6711P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3766
_refine_ls_number_parameters     274
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0839
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_restrained_S_all      1.217
_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
Cu1 Cu 0.04796(5) 0.28954(3) 0.112689(18) 0.01484(12) Uani 1 1 d . . .
Cl1 Cl 0.32654(11) 0.24400(5) 0.07172(4) 0.02152(19) Uani 1 1 d . . .
Cl2 Cl -0.04308(11) 0.38549(5) 0.03210(4) 0.01753(18) Uani 1 1 d . . .
Cl3 Cl -0.06302(13) 0.37294(5) 0.19177(4) 0.0257(2) Uani 1 1 d . . .
Cl4 Cl -0.04665(10) 0.15019(5) 0.14716(3) 0.01566(17) Uani 1 1 d . . .
Cl5 Cl 0.63627(10) 0.58007(5) 0.62209(4) 0.01628(17) Uani 1 1 d . . .
N1 N 1.0478(4) 0.27766(17) 0.34489(12) 0.0146(5) Uani 1 1 d D . .
H1' H 1.123(4) 0.3225(15) 0.3501(17) 0.022 Uiso 1 1 d D . .
N2 N 0.9402(3) 0.13628(17) 0.32670(12) 0.0145(5) Uani 1 1 d . . .
N3 N 1.5626(4) 0.1324(2) 0.21360(13) 0.0239(7) Uani 1 1 d D . .
H3' H 1.663(3) 0.121(3) 0.1940(16) 0.036 Uiso 1 1 d D . .
N4 N 0.7295(4) 0.48176(18) 0.50034(13) 0.0157(6) Uani 1 1 d D . .
H4' H 0.707(5) 0.5244(17) 0.5258(13) 0.024 Uiso 1 1 d D . .
N5 N 0.3471(4) 0.02712(19) 0.42745(13) 0.0196(6) Uani 1 1 d D . .
H5' H 0.250(3) -0.003(2) 0.4381(17) 0.029 Uiso 1 1 d D . .
C1 C 1.0753(4) 0.1971(2) 0.31440(14) 0.0137(6) Uani 1 1 d . . .
C2 C 0.8877(4) 0.2678(2) 0.38025(14) 0.0126(6) Uani 1 1 d . . .
C3 C 0.8219(4) 0.1793(2) 0.36774(14) 0.0129(6) Uani 1 1 d . . .
C4 C 1.2424(4) 0.1774(2) 0.27665(14) 0.0142(6) Uani 1 1 d . . .
C5 C 1.3710(5) 0.2450(2) 0.25913(15) 0.0199(7) Uani 1 1 d . . .
H5 H 1.3479 0.3075 0.2690 0.024 Uiso 1 1 calc R . .
C6 C 1.5330(5) 0.2203(3) 0.22710(15) 0.0235(8) Uani 1 1 d . . .
H6 H 1.6223 0.2657 0.2148 0.028 Uiso 1 1 calc R . .
C7 C 1.4399(5) 0.0655(2) 0.22844(15) 0.0228(7) Uani 1 1 d . . .
H7 H 1.4653 0.0038 0.2168 0.027 Uiso 1 1 calc R . .
C8 C 1.2784(4) 0.0862(2) 0.26029(14) 0.0177(7) Uani 1 1 d . . .
H8 H 1.1912 0.0392 0.2712 0.021 Uiso 1 1 calc R . .
C9 C 0.8301(4) 0.3426(2) 0.42190(14) 0.0133(6) Uani 1 1 d . . .
C10 C 0.8603(4) 0.4342(2) 0.40530(15) 0.0148(6) Uani 1 1 d . . .
H10 H 0.9166 0.4487 0.3663 0.018 Uiso 1 1 calc R . .
C11 C 0.8086(4) 0.5031(2) 0.44548(15) 0.0162(7) Uani 1 1 d . . .
H11 H 0.8287 0.5654 0.4345 0.019 Uiso 1 1 calc R . .
C12 C 0.6983(4) 0.3954(2) 0.51781(15) 0.0157(6) Uani 1 1 d . . .
H12 H 0.6405 0.3833 0.5569 0.019 Uiso 1 1 calc R . .
C13 C 0.7488(4) 0.3239(2) 0.47997(14) 0.0137(6) Uani 1 1 d . . .
H13 H 0.7289 0.2623 0.4930 0.016 Uiso 1 1 calc R . .
C14 C 0.6542(4) 0.1287(2) 0.38960(14) 0.0146(6) Uani 1 1 d . . .
C15 C 0.4904(4) 0.1713(2) 0.41211(14) 0.0147(6) Uani 1 1 d . . .
H15 H 0.4832 0.2363 0.4141 0.018 Uiso 1 1 calc R . .
C16 C 0.3390(4) 0.1184(2) 0.43148(14) 0.0177(7) Uani 1 1 d . . .
H16 H 0.2285 0.1470 0.4477 0.021 Uiso 1 1 calc R . .
C17 C 0.5005(5) -0.0169(2) 0.40536(16) 0.0212(7) Uani 1 1 d . . .
H17 H 0.5010 -0.0820 0.4030 0.025 Uiso 1 1 calc R . .
C18 C 0.6569(4) 0.0322(2) 0.38619(15) 0.0172(7) Uani 1 1 d . . .
H18 H 0.7659 0.0013 0.3708 0.021 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
Cu1 0.0140(2) 0.0131(2) 0.0179(2) -0.00031(15) 0.00608(15) 0.00133(14)
Cl1 0.0157(4) 0.0191(4) 0.0306(4) 0.0034(3) 0.0107(3) 0.0034(3)
Cl2 0.0175(4) 0.0152(4) 0.0204(4) 0.0018(3) 0.0066(3) 0.0045(3)
Cl3 0.0360(5) 0.0186(4) 0.0234(4) -0.0044(3) 0.0120(4) 0.0021(3)
Cl4 0.0135(4) 0.0149(4) 0.0188(4) 0.0003(3) 0.0044(3) -0.0006(3)
Cl5 0.0142(4) 0.0157(4) 0.0192(4) -0.0023(3) 0.0050(3) -0.0028(3)
N1 0.0125(13) 0.0140(13) 0.0174(13) -0.0009(11) 0.0042(11) -0.0030(10)
N2 0.0101(12) 0.0166(13) 0.0170(14) -0.0009(11) 0.0032(10) 0.0004(10)
N3 0.0143(14) 0.0399(18) 0.0181(15) -0.0008(13) 0.0070(11) 0.0062(13)
N4 0.0114(13) 0.0137(13) 0.0221(15) -0.0068(11) 0.0018(11) -0.0005(10)
N5 0.0132(14) 0.0247(16) 0.0212(14) 0.0061(12) 0.0034(11) -0.0090(11)
C1 0.0119(15) 0.0152(15) 0.0141(15) -0.0003(12) 0.0030(12) 0.0008(12)
C2 0.0097(14) 0.0146(15) 0.0137(15) 0.0015(12) 0.0022(12) 0.0024(12)
C3 0.0115(15) 0.0158(15) 0.0116(15) 0.0006(12) 0.0021(12) -0.0006(12)
C4 0.0113(15) 0.0210(16) 0.0100(14) -0.0018(12) -0.0013(12) 0.0008(12)
C5 0.0175(16) 0.0228(17) 0.0194(17) -0.0022(14) 0.0026(13) -0.0026(14)
C6 0.0161(17) 0.036(2) 0.0187(17) 0.0014(15) 0.0037(13) -0.0058(15)
C7 0.0220(18) 0.0278(19) 0.0186(17) -0.0030(14) 0.0025(14) 0.0073(14)
C8 0.0155(16) 0.0208(17) 0.0170(16) -0.0027(13) 0.0033(13) 0.0018(13)
C9 0.0058(14) 0.0161(16) 0.0178(16) -0.0021(12) -0.0004(12) 0.0006(12)
C10 0.0085(14) 0.0175(16) 0.0185(16) 0.0017(13) 0.0015(12) 0.0011(12)
C11 0.0101(15) 0.0133(15) 0.0253(17) 0.0014(13) 0.0025(13) -0.0021(12)
C12 0.0093(14) 0.0200(17) 0.0177(16) 0.0001(13) 0.0001(12) 0.0009(12)
C13 0.0108(14) 0.0130(15) 0.0173(16) 0.0036(12) -0.0009(12) 0.0010(12)
C14 0.0140(15) 0.0181(16) 0.0117(15) 0.0007(12) -0.0006(12) -0.0037(12)
C15 0.0148(15) 0.0160(16) 0.0135(15) -0.0012(12) 0.0021(12) 0.0004(12)
C16 0.0135(16) 0.0250(18) 0.0149(16) 0.0015(13) 0.0036(12) -0.0005(13)
C17 0.0232(18) 0.0165(16) 0.0239(18) 0.0028(14) 0.0008(14) -0.0054(13)
C18 0.0140(16) 0.0170(16) 0.0204(16) -0.0007(13) -0.0007(13) 0.0026(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
Cu1 Cl3 2.2294(9) . ?
Cu1 Cl1 2.2512(8) . ?
Cu1 Cl4 2.2643(8) . ?
Cu1 Cl2 2.2724(9) . ?
N1 C1 1.357(4) . ?
N1 C2 1.372(4) . ?
N2 C1 1.324(4) . ?
N2 C3 1.371(4) . ?
N3 C6 1.330(5) . ?
N3 C7 1.340(5) . ?
N4 C12 1.332(4) . ?
N4 C11 1.340(4) . ?
N5 C16 1.335(4) . ?
N5 C17 1.343(4) . ?
C1 C4 1.463(4) . ?
C2 C3 1.390(4) . ?
C2 C9 1.467(4) . ?
C3 C14 1.468(4) . ?
C4 C5 1.390(4) . ?
C4 C8 1.398(4) . ?
C5 C6 1.384(5) . ?
C7 C8 1.365(4) . ?
C9 C13 1.399(4) . ?
C9 C10 1.398(4) . ?
C10 C11 1.372(4) . ?
C12 C13 1.368(4) . ?
C14 C15 1.396(4) . ?
C14 C18 1.409(4) . ?
C15 C16 1.379(4) . ?
C17 C18 1.375(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
Cl3 Cu1 Cl1 141.09(4) . . ?
Cl3 Cu1 Cl4 97.71(3) . . ?
Cl1 Cu1 Cl4 97.15(3) . . ?
Cl3 Cu1 Cl2 97.58(3) . . ?
Cl1 Cu1 Cl2 96.30(3) . . ?
Cl4 Cu1 Cl2 135.87(3) . . ?
C1 N1 C2 107.5(2) . . ?
C1 N2 C3 105.4(2) . . ?
C6 N3 C7 123.0(3) . . ?
C12 N4 C11 122.4(3) . . ?
C16 N5 C17 122.3(3) . . ?
N2 C1 N1 111.8(3) . . ?
N2 C1 C4 124.1(3) . . ?
N1 C1 C4 124.0(3) . . ?
N1 C2 C3 105.1(3) . . ?
N1 C2 C9 119.8(3) . . ?
C3 C2 C9 135.0(3) . . ?
N2 C3 C2 110.1(3) . . ?
N2 C3 C14 118.2(3) . . ?
C2 C3 C14 131.7(3) . . ?
C5 C4 C8 119.0(3) . . ?
C5 C4 C1 122.6(3) . . ?
C8 C4 C1 118.4(3) . . ?
C6 C5 C4 119.3(3) . . ?
N3 C6 C5 119.5(3) . . ?
N3 C7 C8 119.8(3) . . ?
C7 C8 C4 119.4(3) . . ?
C13 C9 C10 118.5(3) . . ?
C13 C9 C2 120.8(3) . . ?
C10 C9 C2 120.7(3) . . ?
C11 C10 C9 119.8(3) . . ?
N4 C11 C10 119.5(3) . . ?
N4 C12 C13 120.6(3) . . ?
C12 C13 C9 119.1(3) . . ?
C15 C14 C18 118.3(3) . . ?
C15 C14 C3 123.5(3) . . ?
C18 C14 C3 118.2(3) . . ?
C16 C15 C14 119.6(3) . . ?
N5 C16 C15 120.2(3) . . ?
N5 C17 C18 120.1(3) . . ?
C17 C18 C14 119.5(3) . . ?

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
C3 N2 C1 N1 -0.9(3) . . . . ?
C3 N2 C1 C4 174.5(3) . . . . ?
C2 N1 C1 N2 1.4(4) . . . . ?
C2 N1 C1 C4 -174.0(3) . . . . ?
C1 N1 C2 C3 -1.3(3) . . . . ?
C1 N1 C2 C9 176.0(3) . . . . ?
C1 N2 C3 C2 0.0(3) . . . . ?
C1 N2 C3 C14 179.1(3) . . . . ?
N1 C2 C3 N2 0.8(3) . . . . ?
C9 C2 C3 N2 -175.8(3) . . . . ?
N1 C2 C3 C14 -178.1(3) . . . . ?
C9 C2 C3 C14 5.2(6) . . . . ?
N2 C1 C4 C5 173.2(3) . . . . ?
N1 C1 C4 C5 -12.0(5) . . . . ?
N2 C1 C4 C8 -9.9(5) . . . . ?
N1 C1 C4 C8 165.0(3) . . . . ?
C8 C4 C5 C6 -1.3(5) . . . . ?
C1 C4 C5 C6 175.6(3) . . . . ?
C7 N3 C6 C5 1.4(5) . . . . ?
C4 C5 C6 N3 0.1(5) . . . . ?
C6 N3 C7 C8 -1.7(5) . . . . ?
N3 C7 C8 C4 0.4(5) . . . . ?
C5 C4 C8 C7 1.0(5) . . . . ?
C1 C4 C8 C7 -176.0(3) . . . . ?
N1 C2 C9 C13 -144.8(3) . . . . ?
C3 C2 C9 C13 31.5(5) . . . . ?
N1 C2 C9 C10 33.3(4) . . . . ?
C3 C2 C9 C10 -150.4(3) . . . . ?
C13 C9 C10 C11 -0.7(4) . . . . ?
C2 C9 C10 C11 -178.8(3) . . . . ?
C12 N4 C11 C10 0.0(4) . . . . ?
C9 C10 C11 N4 0.0(4) . . . . ?
C11 N4 C12 C13 0.7(5) . . . . ?
N4 C12 C13 C9 -1.3(4) . . . . ?
C10 C9 C13 C12 1.3(4) . . . . ?
C2 C9 C13 C12 179.4(3) . . . . ?
N2 C3 C14 C15 -156.9(3) . . . . ?
C2 C3 C14 C15 22.0(5) . . . . ?
N2 C3 C14 C18 21.5(4) . . . . ?
C2 C3 C14 C18 -159.6(3) . . . . ?
C18 C14 C15 C16 1.4(4) . . . . ?
C3 C14 C15 C16 179.7(3) . . . . ?
C17 N5 C16 C15 0.6(5) . . . . ?
C14 C15 C16 N5 -1.5(5) . . . . ?
C16 N5 C17 C18 0.3(5) . . . . ?
N5 C17 C18 C14 -0.4(5) . . . . ?
C15 C14 C18 C17 -0.5(5) . . . . ?
C3 C14 C18 C17 -178.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.088


data_jcr5zehm
_database_code_depnum_ccdc_archive 'CCDC 873202'
#TrackingRef 'jcr5zehm.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C18 H16 N5), 3(Cl4 Pd), 4(H2 O)'
_chemical_formula_sum            'C36 H40 Cl12 N10 O4 Pd3'
_chemical_formula_weight         1421.38

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.5469(8)
_cell_length_b                   11.5778(12)
_cell_length_c                   14.6595(15)
_cell_angle_alpha                102.136(2)
_cell_angle_beta                 102.265(2)
_cell_angle_gamma                93.705(2)
_cell_volume                     1215.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5732
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      28.31

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_exptl_absorpt_coefficient_mu    1.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_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  '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            11799
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4261
_reflns_number_gt                3878
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_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^)+(0.0298P)^2^+3.2553P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4261
_refine_ls_number_parameters     319
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0810
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.041
_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 0.98668(4) 0.77855(2) 0.71037(2) 0.01309(10) Uani 1 1 d . . .
Pd2 Pd 0.0000 0.5000 1.0000 0.02418(13) Uani 1 2 d S . .
Cl1 Cl 1.29268(12) 0.75742(8) 0.75431(6) 0.0174(2) Uani 1 1 d . . .
Cl2 Cl 1.03973(13) 0.95660(8) 0.82376(7) 0.0181(2) Uani 1 1 d . . .
Cl3 Cl 0.68173(12) 0.79934(8) 0.66535(7) 0.0169(2) Uani 1 1 d . . .
Cl4 Cl 0.94122(14) 0.60064(8) 0.59966(7) 0.0206(2) Uani 1 1 d . . .
Cl5 Cl 0.04416(16) 0.69796(9) 1.08208(7) 0.0288(3) Uani 1 1 d . . .
Cl6 Cl 0.29552(17) 0.50724(10) 0.98718(8) 0.0352(3) Uani 1 1 d . . .
N1 N 0.6416(4) 1.0032(3) 0.3319(2) 0.0158(7) Uani 1 1 d D . .
H1' H 0.654(6) 1.066(2) 0.313(3) 0.024 Uiso 1 1 d D . .
N2 N 0.6721(4) 0.8798(3) 0.4289(2) 0.0178(7) Uani 1 1 d . . .
N3 N 0.9424(5) 1.2660(3) 0.6623(2) 0.0214(8) Uani 1 1 d D . .
H3' H 0.991(6) 1.323(3) 0.708(2) 0.032 Uiso 1 1 d D . .
N4 N 0.3600(5) 0.8551(3) -0.0191(2) 0.0224(8) Uani 1 1 d D . .
H4' H 0.319(6) 0.851(4) -0.0778(8) 0.034 Uiso 1 1 d D . .
N5 N 0.4411(5) 0.4510(3) 0.2996(3) 0.0221(8) Uani 1 1 d D . .
H5' H 0.407(6) 0.3791(12) 0.295(3) 0.033 Uiso 1 1 d D . .
C1 C 0.6980(5) 0.9914(3) 0.4238(3) 0.0164(8) Uani 1 1 d . . .
C2 C 0.5785(5) 0.8935(3) 0.2749(3) 0.0148(8) Uani 1 1 d . . .
C3 C 0.5961(5) 0.8160(3) 0.3368(3) 0.0167(8) Uani 1 1 d . . .
C4 C 0.7792(5) 1.0892(3) 0.5063(3) 0.0172(8) Uani 1 1 d . . .
C5 C 0.8075(6) 1.2061(3) 0.4974(3) 0.0211(9) Uani 1 1 d . . .
H5 H 0.7691 1.2253 0.4369 0.025 Uiso 1 1 calc R . .
C6 C 0.8913(6) 1.2928(4) 0.5767(3) 0.0221(9) Uani 1 1 d . . .
H6 H 0.9133 1.3724 0.5710 0.027 Uiso 1 1 calc R . .
C7 C 0.9157(6) 1.1550(4) 0.6740(3) 0.0239(9) Uani 1 1 d . . .
H7 H 0.9531 1.1390 0.7358 0.029 Uiso 1 1 calc R . .
C8 C 0.8342(6) 1.0645(4) 0.5967(3) 0.0212(9) Uani 1 1 d . . .
H8 H 0.8153 0.9856 0.6046 0.025 Uiso 1 1 calc R . .
C9 C 0.5047(5) 0.8784(3) 0.1711(3) 0.0153(8) Uani 1 1 d . . .
C10 C 0.3876(5) 0.9576(3) 0.1397(3) 0.0179(8) Uani 1 1 d . . .
H10 H 0.3580 1.0209 0.1848 0.021 Uiso 1 1 calc R . .
C11 C 0.3156(6) 0.9438(4) 0.0435(3) 0.0219(9) Uani 1 1 d . . .
H11 H 0.2347 0.9969 0.0214 0.026 Uiso 1 1 calc R . .
C12 C 0.4743(6) 0.7779(4) 0.0076(3) 0.0227(9) Uani 1 1 d . . .
H12 H 0.5026 0.7165 -0.0394 0.027 Uiso 1 1 calc R . .
C13 C 0.5503(6) 0.7883(3) 0.1035(3) 0.0196(9) Uani 1 1 d . . .
H13 H 0.6326 0.7349 0.1233 0.023 Uiso 1 1 calc R . .
C14 C 0.5398(5) 0.6884(3) 0.3212(3) 0.0165(8) Uani 1 1 d . . .
C15 C 0.4197(6) 0.6221(4) 0.2381(3) 0.0219(9) Uani 1 1 d . . .
H15 H 0.3705 0.6591 0.1878 0.026 Uiso 1 1 calc R . .
C16 C 0.3729(6) 0.5032(4) 0.2294(3) 0.0225(9) Uani 1 1 d . . .
H16 H 0.2911 0.4579 0.1728 0.027 Uiso 1 1 calc R . .
C17 C 0.5565(6) 0.5119(4) 0.3811(3) 0.0226(9) Uani 1 1 d . . .
H17 H 0.6029 0.4721 0.4301 0.027 Uiso 1 1 calc R . .
C18 C 0.6073(6) 0.6302(3) 0.3940(3) 0.0196(9) Uani 1 1 d . . .
H18 H 0.6879 0.6732 0.4519 0.023 Uiso 1 1 calc R . .
O31 O 0.7799(4) 0.7645(3) 0.9020(2) 0.0311(7) Uani 1 1 d D . .
H31A H 0.855(6) 0.749(5) 0.948(3) 0.047 Uiso 1 1 d D . .
H31B H 0.842(6) 0.810(4) 0.880(4) 0.047 Uiso 1 1 d D . .
O32 O 0.1391(5) 0.4668(3) 0.7674(2) 0.0361(8) Uani 1 1 d D . .
H32A H 0.152(8) 0.488(5) 0.8270(6) 0.054 Uiso 1 1 d D . .
H32B H 0.112(8) 0.526(3) 0.744(4) 0.054 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.01585(17) 0.01086(16) 0.01175(16) 0.00165(11) 0.00231(12) 0.00164(11)
Pd2 0.0341(3) 0.0178(2) 0.0157(2) 0.00163(18) -0.0022(2) 0.00058(19)
Cl1 0.0173(5) 0.0188(5) 0.0152(5) 0.0026(4) 0.0028(4) 0.0042(4)
Cl2 0.0219(5) 0.0141(5) 0.0155(5) -0.0004(4) 0.0016(4) 0.0022(4)
Cl3 0.0168(5) 0.0150(5) 0.0184(5) 0.0048(4) 0.0023(4) 0.0018(4)
Cl4 0.0271(5) 0.0136(5) 0.0175(5) -0.0009(4) 0.0011(4) 0.0030(4)
Cl5 0.0378(6) 0.0189(5) 0.0231(5) 0.0001(4) -0.0015(5) -0.0001(4)
Cl6 0.0399(7) 0.0299(6) 0.0278(6) -0.0030(5) 0.0014(5) -0.0009(5)
N1 0.0222(18) 0.0117(16) 0.0128(17) 0.0034(13) 0.0024(14) 0.0015(14)
N2 0.0241(18) 0.0160(17) 0.0110(16) 0.0023(13) 0.0003(14) 0.0017(14)
N3 0.028(2) 0.0164(18) 0.0164(18) -0.0010(14) 0.0027(15) -0.0008(15)
N4 0.025(2) 0.0263(19) 0.0122(17) 0.0018(15) 0.0018(15) -0.0057(15)
N5 0.0243(19) 0.0126(17) 0.030(2) 0.0027(16) 0.0104(16) 0.0024(15)
C1 0.020(2) 0.0136(19) 0.016(2) 0.0017(15) 0.0049(16) 0.0030(16)
C2 0.016(2) 0.0129(19) 0.0129(19) 0.0004(15) 0.0016(15) 0.0011(15)
C3 0.016(2) 0.018(2) 0.015(2) 0.0043(16) 0.0009(16) 0.0035(16)
C4 0.019(2) 0.017(2) 0.015(2) 0.0032(16) 0.0031(16) -0.0006(16)
C5 0.030(2) 0.018(2) 0.014(2) 0.0050(16) 0.0025(17) 0.0013(17)
C6 0.030(2) 0.014(2) 0.022(2) 0.0038(17) 0.0059(18) 0.0009(17)
C7 0.033(2) 0.022(2) 0.017(2) 0.0069(17) 0.0033(18) 0.0034(18)
C8 0.031(2) 0.016(2) 0.016(2) 0.0037(16) 0.0035(18) 0.0030(17)
C9 0.016(2) 0.0136(19) 0.0151(19) 0.0028(15) 0.0026(16) -0.0036(15)
C10 0.019(2) 0.0137(19) 0.017(2) -0.0011(16) 0.0026(17) 0.0006(16)
C11 0.023(2) 0.021(2) 0.020(2) 0.0053(17) 0.0034(18) 0.0012(17)
C12 0.025(2) 0.021(2) 0.022(2) -0.0003(17) 0.0109(18) -0.0022(18)
C13 0.023(2) 0.016(2) 0.019(2) 0.0007(16) 0.0046(17) 0.0016(16)
C14 0.019(2) 0.015(2) 0.016(2) 0.0039(16) 0.0058(16) 0.0027(16)
C15 0.026(2) 0.019(2) 0.019(2) 0.0041(17) 0.0006(17) 0.0009(17)
C16 0.024(2) 0.020(2) 0.020(2) 0.0015(17) 0.0038(18) -0.0004(17)
C17 0.032(2) 0.018(2) 0.021(2) 0.0083(17) 0.0066(18) 0.0064(18)
C18 0.026(2) 0.018(2) 0.014(2) 0.0026(16) 0.0039(17) 0.0032(17)
O31 0.0334(19) 0.0362(19) 0.0279(18) 0.0159(15) 0.0082(14) 0.0013(15)
O32 0.057(2) 0.0241(18) 0.0205(17) 0.0023(14) 0.0011(16) -0.0062(16)

_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 Cl4 2.2937(9) . ?
Pd1 Cl3 2.2986(10) . ?
Pd1 Cl1 2.3054(10) . ?
Pd1 Cl2 2.3114(9) . ?
Pd2 Cl6 2.2753(13) 2_567 ?
Pd2 Cl6 2.2753(13) . ?
Pd2 Cl5 2.3202(10) . ?
Pd2 Cl5 2.3202(10) 2_567 ?
N1 C2 1.358(5) . ?
N1 C1 1.362(5) . ?
N2 C1 1.314(5) . ?
N2 C3 1.376(5) . ?
N3 C6 1.340(5) . ?
N3 C7 1.340(5) . ?
N4 C11 1.336(5) . ?
N4 C12 1.342(6) . ?
N5 C16 1.329(6) . ?
N5 C17 1.345(5) . ?
C1 C4 1.463(5) . ?
C2 C3 1.398(5) . ?
C2 C9 1.474(5) . ?
C3 C14 1.467(5) . ?
C4 C5 1.393(5) . ?
C4 C8 1.397(6) . ?
C5 C6 1.370(6) . ?
C7 C8 1.372(6) . ?
C9 C10 1.394(5) . ?
C9 C13 1.395(5) . ?
C10 C11 1.371(6) . ?
C12 C13 1.377(6) . ?
C14 C15 1.394(5) . ?
C14 C18 1.402(6) . ?
C15 C16 1.371(6) . ?
C17 C18 1.361(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
Cl4 Pd1 Cl3 89.80(4) . . ?
Cl4 Pd1 Cl1 89.93(3) . . ?
Cl3 Pd1 Cl1 179.56(3) . . ?
Cl4 Pd1 Cl2 178.53(4) . . ?
Cl3 Pd1 Cl2 91.63(3) . . ?
Cl1 Pd1 Cl2 88.65(3) . . ?
Cl6 Pd2 Cl6 180.0 2_567 . ?
Cl6 Pd2 Cl5 88.80(4) 2_567 . ?
Cl6 Pd2 Cl5 91.20(4) . . ?
Cl6 Pd2 Cl5 91.20(4) 2_567 2_567 ?
Cl6 Pd2 Cl5 88.80(4) . 2_567 ?
Cl5 Pd2 Cl5 180.0 . 2_567 ?
C2 N1 C1 108.2(3) . . ?
C1 N2 C3 106.3(3) . . ?
C6 N3 C7 122.1(3) . . ?
C11 N4 C12 123.0(4) . . ?
C16 N5 C17 121.7(4) . . ?
N2 C1 N1 111.1(3) . . ?
N2 C1 C4 124.0(4) . . ?
N1 C1 C4 124.9(3) . . ?
N1 C2 C3 105.3(3) . . ?
N1 C2 C9 120.6(3) . . ?
C3 C2 C9 134.1(3) . . ?
N2 C3 C2 109.1(3) . . ?
N2 C3 C14 118.5(3) . . ?
C2 C3 C14 132.2(4) . . ?
C5 C4 C8 118.8(4) . . ?
C5 C4 C1 122.1(4) . . ?
C8 C4 C1 119.1(4) . . ?
C6 C5 C4 119.3(4) . . ?
N3 C6 C5 120.3(4) . . ?
N3 C7 C8 119.9(4) . . ?
C7 C8 C4 119.5(4) . . ?
C10 C9 C13 119.2(4) . . ?
C10 C9 C2 118.8(3) . . ?
C13 C9 C2 122.0(4) . . ?
C11 C10 C9 119.6(4) . . ?
N4 C11 C10 119.5(4) . . ?
N4 C12 C13 119.6(4) . . ?
C12 C13 C9 119.1(4) . . ?
C15 C14 C18 118.1(4) . . ?
C15 C14 C3 123.3(4) . . ?
C18 C14 C3 118.6(3) . . ?
C16 C15 C14 119.7(4) . . ?
N5 C16 C15 120.5(4) . . ?
N5 C17 C18 120.4(4) . . ?
C17 C18 C14 119.6(4) . . ?

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
C3 N2 C1 N1 0.1(4) . . . . ?
C3 N2 C1 C4 -179.1(4) . . . . ?
C2 N1 C1 N2 -0.8(5) . . . . ?
C2 N1 C1 C4 178.4(4) . . . . ?
C1 N1 C2 C3 1.2(4) . . . . ?
C1 N1 C2 C9 178.9(3) . . . . ?
C1 N2 C3 C2 0.6(4) . . . . ?
C1 N2 C3 C14 -175.7(3) . . . . ?
N1 C2 C3 N2 -1.1(4) . . . . ?
C9 C2 C3 N2 -178.4(4) . . . . ?
N1 C2 C3 C14 174.6(4) . . . . ?
C9 C2 C3 C14 -2.7(8) . . . . ?
N2 C1 C4 C5 178.7(4) . . . . ?
N1 C1 C4 C5 -0.4(6) . . . . ?
N2 C1 C4 C8 0.2(6) . . . . ?
N1 C1 C4 C8 -178.9(4) . . . . ?
C8 C4 C5 C6 1.3(6) . . . . ?
C1 C4 C5 C6 -177.2(4) . . . . ?
C7 N3 C6 C5 0.5(6) . . . . ?
C4 C5 C6 N3 -1.2(6) . . . . ?
C6 N3 C7 C8 0.3(6) . . . . ?
N3 C7 C8 C4 -0.2(6) . . . . ?
C5 C4 C8 C7 -0.6(6) . . . . ?
C1 C4 C8 C7 178.0(4) . . . . ?
N1 C2 C9 C10 -43.6(5) . . . . ?
C3 C2 C9 C10 133.3(5) . . . . ?
N1 C2 C9 C13 135.6(4) . . . . ?
C3 C2 C9 C13 -47.5(6) . . . . ?
C13 C9 C10 C11 1.8(6) . . . . ?
C2 C9 C10 C11 -179.0(4) . . . . ?
C12 N4 C11 C10 -0.5(6) . . . . ?
C9 C10 C11 N4 -0.6(6) . . . . ?
C11 N4 C12 C13 0.4(6) . . . . ?
N4 C12 C13 C9 0.8(6) . . . . ?
C10 C9 C13 C12 -1.9(6) . . . . ?
C2 C9 C13 C12 179.0(4) . . . . ?
N2 C3 C14 C15 162.2(4) . . . . ?
C2 C3 C14 C15 -13.2(7) . . . . ?
N2 C3 C14 C18 -16.7(5) . . . . ?
C2 C3 C14 C18 168.0(4) . . . . ?
C18 C14 C15 C16 -0.7(6) . . . . ?
C3 C14 C15 C16 -179.6(4) . . . . ?
C17 N5 C16 C15 0.4(6) . . . . ?
C14 C15 C16 N5 0.1(6) . . . . ?
C16 N5 C17 C18 -0.1(6) . . . . ?
N5 C17 C18 C14 -0.6(6) . . . . ?
C15 C14 C18 C17 0.9(6) . . . . ?
C3 C14 C18 C17 179.9(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.106