Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2006

data_global

_journal_coden_Cambridge         1350

_publ_requested_journal          CrystEngComm

loop_
_publ_author_name
'Fiorenzo Zordan'
'Guillermo Minguez Espallargas'
'Lee Brammer'

_publ_contact_author_name        'Lee Brammer'
_publ_contact_author_address     
;
Department of Chemistry
University of Sheffield
Brook Hill
Sheffield
S3 7HF
UNITED KINGDOM
;

_publ_contact_author_email       'LEE.BRAMMER@SHEFFIELD.AC.UK '

_publ_section_title              
;
Unexpected structural homologies involving hydrogen-bonded and
halogen-bonded networks in halopyridinium halometallate salts
;

# Compound 1

data_ilb173m
_database_code_depnum_ccdc_archive 'CCDC 299026'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C5 H5 Cl N), Cl4 Pd'
_chemical_formula_sum            'C10 H10 Cl6 N2 Pd'
_chemical_formula_weight         477.30

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   6.9605(14)
_cell_length_b                   7.3662(15)
_cell_length_c                   8.6496(17)
_cell_angle_alpha                113.41(3)
_cell_angle_beta                 91.97(3)
_cell_angle_gamma                98.06(3)
_cell_volume                     400.97(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2192
_cell_measurement_theta_min      2.9745
_cell_measurement_theta_max      28.2945

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             232
_exptl_absorpt_coefficient_mu    2.142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5659
_exptl_absorpt_correction_T_max  0.7394
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'medium focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2933
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         28.40
_reflns_number_total             1727
_reflns_number_gt                1581
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.1098P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1727
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1518
_refine_ls_wR_factor_gt          0.1497
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_restrained_S_all      1.163
_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
Pd1 Pd 0.0000 0.0000 0.0000 0.0225(2) Uani 1 2 d S . .
Cl1 Cl -0.35529(19) 0.69709(17) 0.4880(2) 0.0401(4) Uani 1 1 d . . .
Cl2 Cl -0.10630(16) 0.25984(15) 0.21422(14) 0.0291(3) Uani 1 1 d . . .
Cl3 Cl -0.21056(17) -0.22711(16) 0.06344(16) 0.0341(3) Uani 1 1 d . . .
N1 N -0.2128(6) 1.3516(6) 0.7719(5) 0.0284(9) Uani 1 1 d . . .
H1 H -0.1795 1.4820 0.8300 0.034 Uiso 1 1 calc R . .
C2 C -0.3104(7) 1.2436(8) 0.8461(7) 0.0320(10) Uani 1 1 d . . .
H2 H -0.3456 1.3081 0.9578 0.038 Uiso 1 1 calc R . .
C3 C -0.3595(7) 1.0397(8) 0.7604(7) 0.0328(11) Uani 1 1 d . . .
H3 H -0.4286 0.9601 0.8107 0.039 Uiso 1 1 calc R . .
C4 C -0.3048(6) 0.9532(7) 0.5976(7) 0.0287(10) Uani 1 1 d . . .
C5 C -0.2105(6) 1.0683(7) 0.5212(6) 0.0266(9) Uani 1 1 d . . .
H5 H -0.1793 1.0085 0.4077 0.032 Uiso 1 1 calc R . .
C6 C -0.1633(7) 1.2711(7) 0.6137(6) 0.0275(9) Uani 1 1 d . . .
H6 H -0.0957 1.3542 0.5658 0.033 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0238(3) 0.0186(3) 0.0222(3) 0.0063(2) 0.00105(19) 0.0013(2)
Cl1 0.0384(7) 0.0204(6) 0.0548(9) 0.0112(6) -0.0063(6) -0.0007(5)
Cl2 0.0354(6) 0.0217(5) 0.0273(6) 0.0069(5) 0.0072(5) 0.0035(4)
Cl3 0.0390(6) 0.0215(5) 0.0347(7) 0.0058(5) 0.0107(5) -0.0018(5)
N1 0.0293(18) 0.0217(19) 0.030(2) 0.0065(17) -0.0004(16) 0.0026(15)
C2 0.031(2) 0.037(3) 0.025(2) 0.010(2) 0.0007(18) 0.006(2)
C3 0.029(2) 0.034(3) 0.037(3) 0.019(2) 0.0001(19) 0.000(2)
C4 0.022(2) 0.0194(19) 0.037(3) 0.005(2) -0.0031(18) 0.0013(16)
C5 0.024(2) 0.025(2) 0.028(3) 0.008(2) 0.0027(17) 0.0054(17)
C6 0.029(2) 0.025(2) 0.028(3) 0.009(2) 0.0024(18) 0.0037(17)

_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 Cl2 2.3060(14) 2 ?
Pd1 Cl2 2.3060(14) . ?
Pd1 Cl3 2.3119(13) 2 ?
Pd1 Cl3 2.3119(13) . ?
Cl1 C4 1.718(5) . ?
N1 C6 1.336(6) . ?
N1 C2 1.338(7) . ?
C2 C3 1.370(7) . ?
C3 C4 1.388(7) . ?
C4 C5 1.380(7) . ?
C5 C6 1.369(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
Cl2 Pd1 Cl2 180.00(5) 2 . ?
Cl2 Pd1 Cl3 89.56(5) 2 2 ?
Cl2 Pd1 Cl3 90.44(5) . 2 ?
Cl2 Pd1 Cl3 90.44(5) 2 . ?
Cl2 Pd1 Cl3 89.56(5) . . ?
Cl3 Pd1 Cl3 180.00(6) 2 . ?
C6 N1 C2 123.2(4) . . ?
N1 C2 C3 119.7(5) . . ?
C2 C3 C4 117.8(5) . . ?
C5 C4 C3 121.5(4) . . ?
C5 C4 Cl1 119.0(4) . . ?
C3 C4 Cl1 119.5(4) . . ?
C6 C5 C4 118.1(4) . . ?
N1 C6 C5 119.7(5) . . ?

_diffrn_measured_fraction_theta_max 0.857
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.250
_refine_diff_density_min         -2.642
_refine_diff_density_rms         0.194

#END

# Compound 2

data_ilb91m
_database_code_depnum_ccdc_archive 'CCDC 299027'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl8 Cu3, 2(C5 H5 Cl N)'
_chemical_formula_sum            'C10 H10 Cl10 Cu3 N2'
_chemical_formula_weight         703.32

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   3.8783(9)
_cell_length_b                   11.217(3)
_cell_length_c                   12.564(3)
_cell_angle_alpha                103.511(4)
_cell_angle_beta                 93.340(5)
_cell_angle_gamma                99.507(4)
_cell_volume                     521.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1375
_cell_measurement_theta_min      3.754
_cell_measurement_theta_max      23.193

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             341
_exptl_absorpt_coefficient_mu    4.311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4120
_exptl_absorpt_correction_T_max  0.6976
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'medium-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3026
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         26.36
_reflns_number_total             2082
_reflns_number_gt                1639
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.1409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2082
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0726
_refine_ls_wR_factor_ref         0.2084
_refine_ls_wR_factor_gt          0.1985
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_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
Cu1 Cu 0.5000 0.0000 0.0000 0.0194(4) Uani 1 2 d S . .
Cu2 Cu 0.74527(18) -0.13160(6) -0.24827(6) 0.0191(3) Uani 1 1 d . . .
Cl3 Cl 0.3833(4) -0.19176(13) -0.12253(13) 0.0212(4) Uani 1 1 d . . .
Cl4 Cl 0.8826(4) 0.06054(13) -0.11625(12) 0.0192(4) Uani 1 1 d . . .
Cl5 Cl 1.1286(4) -0.05577(13) -0.35474(13) 0.0236(4) Uani 1 1 d . . .
Cl6 Cl 0.6306(4) -0.32363(12) -0.36302(13) 0.0214(4) Uani 1 1 d . . .
N1 N 1.0935(12) -0.2882(4) -0.5630(4) 0.0226(11) Uani 1 1 d . . .
H1 H 1.0448 -0.2658 -0.4945 0.027 Uiso 1 1 calc R . .
C2 C 0.9740(16) -0.4072(6) -0.6218(6) 0.0261(14) Uani 1 1 d . . .
H2 H 0.8399 -0.4650 -0.5888 0.031 Uiso 1 1 calc R . .
C3 C 1.0459(16) -0.4444(6) -0.7287(6) 0.0288(15) Uani 1 1 d . . .
H3 H 0.9608 -0.5273 -0.7709 0.035 Uiso 1 1 calc R . .
C4 C 1.2462(14) -0.3580(5) -0.7735(5) 0.0217(12) Uani 1 1 d . . .
Cl1 Cl 1.3441(5) -0.39999(18) -0.90686(15) 0.0410(5) Uani 1 1 d . . .
C5 C 1.3674(15) -0.2365(5) -0.7123(5) 0.0234(13) Uani 1 1 d . . .
H5 H 1.5054 -0.1775 -0.7432 0.028 Uiso 1 1 calc R . .
C6 C 1.2836(16) -0.2035(5) -0.6063(5) 0.0230(13) Uani 1 1 d . . .
H6 H 1.3603 -0.1204 -0.5634 0.028 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 0.0174(6) 0.0224(6) 0.0170(7) 0.0034(5) 0.0085(5) -0.0002(4)
Cu2 0.0182(5) 0.0195(5) 0.0180(5) 0.0024(3) 0.0088(3) -0.0006(3)
Cl3 0.0196(8) 0.0221(8) 0.0202(9) 0.0037(6) 0.0087(6) -0.0010(5)
Cl4 0.0178(7) 0.0214(7) 0.0178(8) 0.0046(6) 0.0077(6) 0.0006(5)
Cl5 0.0260(8) 0.0211(7) 0.0214(9) 0.0021(6) 0.0138(6) -0.0016(5)
Cl6 0.0188(7) 0.0195(7) 0.0234(9) 0.0020(6) 0.0065(6) 0.0003(5)
N1 0.020(2) 0.027(3) 0.021(3) 0.006(2) 0.011(2) 0.0021(19)
C2 0.024(3) 0.027(3) 0.029(4) 0.012(3) 0.003(3) 0.001(2)
C3 0.023(3) 0.023(3) 0.038(4) 0.003(3) -0.005(3) 0.005(2)
C4 0.017(3) 0.025(3) 0.023(3) 0.002(3) 0.008(2) 0.007(2)
Cl1 0.0365(10) 0.0589(11) 0.0215(10) -0.0050(8) 0.0088(7) 0.0116(8)
C5 0.025(3) 0.021(3) 0.027(4) 0.011(3) 0.010(3) 0.006(2)
C6 0.028(3) 0.022(3) 0.021(3) 0.008(3) 0.006(3) 0.006(2)

_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 Cl4 2.2758(14) . ?
Cu1 Cl4 2.2758(14) 2_655 ?
Cu1 Cl3 2.2916(15) . ?
Cu1 Cl3 2.2916(15) 2_655 ?
Cu2 Cl5 2.2514(15) . ?
Cu2 Cl6 2.2526(15) . ?
Cu2 Cl3 2.3163(16) . ?
Cu2 Cl4 2.3511(16) . ?
N1 C6 1.341(7) . ?
N1 C2 1.356(8) . ?
N1 H1 0.8800 . ?
C2 C3 1.369(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(8) . ?
C4 Cl1 1.714(6) . ?
C5 C6 1.369(9) . ?
C5 H5 0.9500 . ?
C6 H6 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
Cl4 Cu1 Cl4 180.00(5) . 2_655 ?
Cl4 Cu1 Cl3 86.72(5) . . ?
Cl4 Cu1 Cl3 93.28(5) 2_655 . ?
Cl4 Cu1 Cl3 93.28(5) . 2_655 ?
Cl4 Cu1 Cl3 86.72(5) 2_655 2_655 ?
Cl3 Cu1 Cl3 180.00(10) . 2_655 ?
Cl5 Cu2 Cl6 93.05(6) . . ?
Cl5 Cu2 Cl3 173.59(6) . . ?
Cl6 Cu2 Cl3 92.84(6) . . ?
Cl5 Cu2 Cl4 89.52(6) . . ?
Cl6 Cu2 Cl4 174.85(6) . . ?
Cl3 Cu2 Cl4 84.41(6) . . ?
Cu1 Cl3 Cu2 94.62(5) . . ?
Cu1 Cl4 Cu2 94.10(5) . . ?
C6 N1 C2 121.9(6) . . ?
C6 N1 H1 119.0 . . ?
C2 N1 H1 119.0 . . ?
N1 C2 C3 120.2(6) . . ?
N1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 118.2(6) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C3 C4 C5 121.0(6) . . ?
C3 C4 Cl1 120.0(5) . . ?
C5 C4 Cl1 119.0(5) . . ?
C6 C5 C4 118.5(6) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
N1 C6 C5 120.1(6) . . ?
N1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl4 Cu1 Cl3 Cu2 -3.03(5) . . . . ?
Cl4 Cu1 Cl3 Cu2 176.97(5) 2_655 . . . ?
Cl3 Cu1 Cl3 Cu2 75(100) 2_655 . . . ?
Cl5 Cu2 Cl3 Cu1 21.9(5) . . . . ?
Cl6 Cu2 Cl3 Cu1 178.58(5) . . . . ?
Cl4 Cu2 Cl3 Cu1 2.94(5) . . . . ?
Cl4 Cu1 Cl4 Cu2 38(30) 2_655 . . . ?
Cl3 Cu1 Cl4 Cu2 2.99(5) . . . . ?
Cl3 Cu1 Cl4 Cu2 -177.01(5) 2_655 . . . ?
Cl5 Cu2 Cl4 Cu1 179.11(5) . . . . ?
Cl6 Cu2 Cl4 Cu1 -60.8(6) . . . . ?
Cl3 Cu2 Cl4 Cu1 -2.96(5) . . . . ?
C6 N1 C2 C3 0.0(9) . . . . ?
N1 C2 C3 C4 0.9(9) . . . . ?
C2 C3 C4 C5 -0.8(9) . . . . ?
C2 C3 C4 Cl1 179.9(4) . . . . ?
C3 C4 C5 C6 -0.2(9) . . . . ?
Cl1 C4 C5 C6 179.1(5) . . . . ?
C2 N1 C6 C5 -1.0(9) . . . . ?
C4 C5 C6 N1 1.1(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.600
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.288

#END

# Compound 3

data_ilb292t
_database_code_depnum_ccdc_archive 'CCDC 299028'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C5 H5 Br N), Cl6 Pt'
_chemical_formula_sum            'C10 H10 Br2 Cl6 N2 Pt'
_chemical_formula_weight         725.81

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   8.5802(10)
_cell_length_b                   16.7418(19)
_cell_length_c                   7.0007(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.504(2)
_cell_angle_gamma                90.00
_cell_volume                     929.06(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4673
_cell_measurement_theta_min      2.8405
_cell_measurement_theta_max      27.7685

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             668
_exptl_absorpt_coefficient_mu    12.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1022
_exptl_absorpt_correction_T_max  0.2889
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'medium focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7685
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         27.91
_reflns_number_total             2109
_reflns_number_gt                1879
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.1029P)^2^+12.4504P] 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         2109
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.1685
_refine_ls_wR_factor_gt          0.1651
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.137
_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 0.0000 0.0000 0.0000 0.0206(2) Uani 1 2 d S . .
Cl1 Cl 0.0455(3) -0.12660(12) 0.1620(3) 0.0164(4) Uani 1 1 d . . .
Cl2 Cl 0.0998(3) -0.05210(12) -0.2503(3) 0.0151(4) Uani 1 1 d . . .
Cl3 Cl 0.2798(3) 0.03700(13) 0.2088(3) 0.0167(4) Uani 1 1 d . . .
N1 N 0.2364(10) 0.1155(5) -0.3740(13) 0.0171(15) Uani 1 1 d . . .
H1 H 0.1576 0.0787 -0.4210 0.021 Uiso 1 1 calc R . .
C2 C 0.1939(12) 0.1919(6) -0.4240(14) 0.0175(18) Uani 1 1 d . . .
H2 H 0.0808 0.2055 -0.5080 0.021 Uiso 1 1 calc R . .
C3 C 0.3132(11) 0.2500(6) -0.3543(14) 0.0158(17) Uani 1 1 d . . .
H3 H 0.2852 0.3045 -0.3891 0.019 Uiso 1 1 calc R . .
C4 C 0.4783(12) 0.2276(6) -0.2297(13) 0.0158(17) Uani 1 1 d . . .
Br1 Br 0.64537(12) 0.30605(6) -0.12607(16) 0.0228(3) Uani 1 1 d . . .
C5 C 0.5198(12) 0.1485(6) -0.1792(15) 0.0172(17) Uani 1 1 d . . .
H5 H 0.6315 0.1330 -0.0947 0.021 Uiso 1 1 calc R . .
C6 C 0.3920(13) 0.0928(6) -0.2568(15) 0.0193(18) Uani 1 1 d . . .
H6 H 0.4157 0.0378 -0.2260 0.023 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
Pt1 0.0182(3) 0.0206(3) 0.0214(3) 0.00063(18) 0.0058(2) 0.00066(17)
Cl1 0.0143(10) 0.0153(10) 0.0183(10) 0.0051(8) 0.0047(8) 0.0039(7)
Cl2 0.0135(10) 0.0161(10) 0.0137(9) -0.0009(7) 0.0029(8) 0.0005(7)
Cl3 0.0103(10) 0.0162(10) 0.0207(10) -0.0037(8) 0.0026(8) -0.0011(7)
N1 0.013(4) 0.018(4) 0.019(4) -0.004(3) 0.005(3) -0.005(3)
C2 0.014(4) 0.018(4) 0.015(4) 0.000(3) -0.001(4) 0.002(3)
C3 0.011(4) 0.019(4) 0.016(4) -0.001(3) 0.004(3) -0.001(3)
C4 0.015(4) 0.022(4) 0.012(4) -0.001(3) 0.007(3) 0.000(3)
Br1 0.0171(5) 0.0212(5) 0.0274(5) -0.0053(4) 0.0054(4) -0.0084(3)
C5 0.011(4) 0.019(4) 0.019(4) -0.001(3) 0.002(4) -0.001(3)
C6 0.023(5) 0.014(4) 0.022(5) 0.001(4) 0.010(4) 0.000(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
Pt1 Cl1 2.365(2) . ?
Pt1 Cl1 2.365(2) 3 ?
Pt1 Cl3 2.366(2) 3 ?
Pt1 Cl3 2.366(2) . ?
Pt1 Cl2 2.390(2) . ?
Pt1 Cl2 2.390(2) 3 ?
N1 C6 1.327(13) . ?
N1 C2 1.340(12) . ?
C2 C3 1.360(13) . ?
C3 C4 1.401(13) . ?
C4 C5 1.382(13) . ?
C4 Br1 1.874(10) . ?
C5 C6 1.382(13) . ?

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
Cl1 Pt1 Cl1 180.00(12) . 3 ?
Cl1 Pt1 Cl3 90.23(8) . 3 ?
Cl1 Pt1 Cl3 89.77(8) 3 3 ?
Cl1 Pt1 Cl3 89.77(8) . . ?
Cl1 Pt1 Cl3 90.23(8) 3 . ?
Cl3 Pt1 Cl3 180.00(12) 3 . ?
Cl1 Pt1 Cl2 89.13(7) . . ?
Cl1 Pt1 Cl2 90.87(7) 3 . ?
Cl3 Pt1 Cl2 90.85(7) 3 . ?
Cl3 Pt1 Cl2 89.15(7) . . ?
Cl1 Pt1 Cl2 90.87(7) . 3 ?
Cl1 Pt1 Cl2 89.13(7) 3 3 ?
Cl3 Pt1 Cl2 89.15(7) 3 3 ?
Cl3 Pt1 Cl2 90.85(7) . 3 ?
Cl2 Pt1 Cl2 180.00(8) . 3 ?
C6 N1 C2 122.9(8) . . ?
N1 C2 C3 119.8(9) . . ?
C2 C3 C4 118.3(9) . . ?
C5 C4 C3 121.1(9) . . ?
C5 C4 Br1 119.3(7) . . ?
C3 C4 Br1 119.7(7) . . ?
C4 C5 C6 117.2(9) . . ?
N1 C6 C5 120.6(9) . . ?

_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        27.91
_diffrn_measured_fraction_theta_full 0.947
_refine_diff_density_max         3.221
_refine_diff_density_min         -3.274
_refine_diff_density_rms         0.362

#END


