Supplementary Material (ESI) for PCCP
This journal is © The Owner Societies 2001

data_global

_audit_creation_method           SHELXL-97

# PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic     ?
_journal_date_from_coeditor       ?
_journal_date_accepted            ?
_journal_coeditor_code            ?

# SUBMISSION DETAILS

_publ_contact_author_name         'Jacek Zaleski'
_publ_contact_author_address
; Institute of Chemistry
  University of Opole
  Oleska 48
  45-052 Opole
  Poland
;
_publ_contact_author_email        zaleski@uni.opole.pl

_publ_contact_letter
;
 ?
;
_publ_requested_journal            ''
_publ_requested_category                  FO
_publ_requested_coeditor           ''

# TITLE AND AUTHOR LIST

_publ_section_title
;
 ? 
;

loop_
_publ_author_name
_publ_author_address
 'Zaleski, Jacek'
;Institute of Chemistry
 University of Opole
 Oleska 48
 45-052 Opole
 Poland
;
 ''
;Institute of Chemistry
 University of Wroc\%law
 Poland
;
 ''
;Institute of Chemistry
 University of 
 
 Poland
;
# TEXT

_publ_section_abstract
; 

;
_publ_section_comment
;
;
_publ_section_acknowledgements
;
;
_publ_section_references
;

KUMA, (1997). KUMA Diffraction Software, ver. KM4b8, Wroc\/law, Poland. 

Sheldrick, G. M. (1990). SHELXTL. Siemens Analytical X--ray Instrument Inc., 
Madison, Winsconsin, USA. 
 
Sheldrick, G. M. (1997). SHELXL97. Program for the Refinement of Crystal 
Structures. 

;
_publ_section_figure_captions 
;
 
;
_publ_section_exptl_prep
;

;

#############################################################################
 
data_p1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C10 H12 Bi2 Cl8 N2' 
_chemical_formula_weight          861.78 
 
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' 
 'Bi'  'Bi'  -4.1077  10.2566 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'Monoclinic' 
_symmetry_space_group_name_H-M    'Cc' 
 
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' 
 
_cell_length_a                    12.717(3) 
_cell_length_b                    12.894(3) 
_cell_length_c                    7.274(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  118.49(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      1048.3(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     28 
_cell_measurement_theta_min       8 
_cell_measurement_theta_max       15 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.2 
_exptl_crystal_size_min           0.2 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.730 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              776 
_exptl_absorpt_coefficient_mu     17.778 
_exptl_absorpt_correction_type    'semiempirical' 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   'KUMA KM4 diffractometer'
_diffrn_measurement_method        \w
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          2
_diffrn_standards_interval_count  50
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         2.24  
_diffrn_reflns_number             1688 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0244 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -8 
_diffrn_reflns_limit_l_max        7 
_diffrn_reflns_theta_min          2.41 
_diffrn_reflns_theta_max          25.19 
_reflns_number_total              1688 
_reflns_number_gt                 1504 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_cell_refinement
   'KUMA Diffraction Software, ver. KM4b8 (KUMA, 1997)'
_computing_data_reduction
   'KUMA Diffraction Software, datared9 (KUMA, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 1990)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'
 
_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 w=1/[\s^2^(Fo^2^)+(0.0471P)^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     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00488(17) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.00 
_refine_ls_number_reflns          1688 
_refine_ls_number_parameters      101 
_refine_ls_number_restraints      75 
_refine_ls_R_factor_all           0.0340 
_refine_ls_R_factor_gt            0.0268 
_refine_ls_wR_factor_ref          0.0718 
_refine_ls_wR_factor_gt           0.0693 
_refine_ls_goodness_of_fit_ref    1.129 
_refine_ls_restrained_S_all       1.120 
_refine_ls_shift/su_max           0.008 
_refine_ls_shift/su_mean          0.001 
 
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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Bi1 Bi 0.9982(3) 0.085389(18) 0.2468(5) 0.03320(8) Uani 1 d U . . 
Cl1 Cl 1.1334(4) 0.0878(3) 0.6699(6) 0.0681(17) Uani 1 d U . . 
Cl2 Cl 0.8641(2) 0.0784(3) -0.1757(3) 0.0378(9) Uani 1 d U . . 
Cl3 Cl 1.1378(3) 0.2121(4) 0.2313(6) 0.0618(13) Uani 1 d U . . 
Cl4 Cl 0.8638(3) 0.2193(3) 0.2769(6) 0.0582(13) Uani 1 d U . . 
N1 N 1.0340(7) 0.3306(7) -0.239(2) 0.070(4) Uani 1 d DU . . 
H1A H 1.0614 0.2653 -0.2275 0.080 Uiso 1 d R . . 
C2 C 0.9169(10) 0.3492(9) -0.283(2) 0.065(3) Uani 1 d DU . . 
H2A H 0.8583 0.2970 -0.3050 0.080 Uiso 1 d R . . 
C3 C 0.8870(11) 0.4517(8) -0.303(2) 0.068(3) Uani 1 d DU . . 
H3A H 0.8060 0.4715 -0.3435 0.080 Uiso 1 d R . . 
C4 C 0.9685(8) 0.5284(10) -0.255(2) 0.070(4) Uani 1 d DU . . 
H4A H 0.9400 0.5978 -0.2601 0.080 Uiso 1 d R . . 
C5 C 1.0784(10) 0.5109(9) -0.230(3) 0.073(4) Uani 1 d DU . . 
H5A H 1.1281 0.5713 -0.2005 0.080 Uiso 1 d R . . 
C6 C 1.1103(12) 0.4112(8) -0.211(3) 0.065(4) Uani 1 d DU . . 
H6A H 1.1906 0.4038 -0.1893 0.080 Uiso 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 
Bi1 0.03300(12) 0.03327(13) 0.03297(13) -0.0017(5) 0.01544(9) -0.0007(5) 
Cl1 0.060(2) 0.070(3) 0.048(2) 0.0057(17) 0.0043(19) -0.0049(19) 
Cl2 0.0350(15) 0.0388(16) 0.0402(16) -0.0019(12) 0.0184(13) 0.0147(12) 
Cl3 0.0584(18) 0.068(2) 0.058(2) -0.0038(17) 0.0267(16) -0.0149(18) 
Cl4 0.062(2) 0.0453(19) 0.065(2) -0.0083(16) 0.0284(18) 0.0223(16) 
N1 0.075(6) 0.051(4) 0.070(6) 0.019(5) 0.024(8) 0.020(4) 
C2 0.074(6) 0.080(6) 0.054(6) 0.007(7) 0.041(6) -0.005(6) 
C3 0.071(5) 0.083(7) 0.051(6) -0.011(7) 0.030(5) 0.027(5) 
C4 0.097(7) 0.070(6) 0.059(6) 0.025(6) 0.052(8) 0.031(5) 
C5 0.085(7) 0.061(5) 0.068(8) 0.029(7) 0.033(7) 0.010(6) 
C6 0.056(6) 0.070(7) 0.059(8) -0.015(7) 0.020(6) 0.006(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 
Bi1 Cl3 2.454(5) . ? 
Bi1 Cl4 2.512(5) . ? 
Bi1 Cl2 2.714(4) . ? 
Bi1 Cl1 2.717(6) . ? 
Bi1 Cl2 2.933(4) 2 ? 
Bi1 Cl1 3.029(6) 2_554 ? 
Cl1 Bi1 3.029(6) 2 ? 
Cl2 Bi1 2.933(4) 2_554 ? 
N1 C6 1.368(11) . ? 
N1 C2 1.387(11) . ? 
C2 C3 1.364(12) . ? 
C3 C4 1.352(12) . ? 
C4 C5 1.339(12) . ? 
C5 C6 1.336(11) . ? 
 
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 Bi1 Cl4 94.79(10) . . ? 
Cl3 Bi1 Cl2 92.72(16) . . ? 
Cl4 Bi1 Cl2 92.02(14) . . ? 
Cl3 Bi1 Cl1 87.93(17) . . ? 
Cl4 Bi1 Cl1 89.00(18) . . ? 
Cl2 Bi1 Cl1 178.74(8) . . ? 
Cl3 Bi1 Cl2 171.01(16) . 2 ? 
Cl4 Bi1 Cl2 89.77(17) . 2 ? 
Cl2 Bi1 Cl2 94.86(11) . 2 ? 
Cl1 Bi1 Cl2 84.40(15) . 2 ? 
Cl3 Bi1 Cl1 89.77(19) . 2_554 ? 
Cl4 Bi1 Cl1 173.14(16) . 2_554 ? 
Cl2 Bi1 Cl1 82.63(13) . 2_554 ? 
Cl1 Bi1 Cl1 96.30(15) . 2_554 ? 
Cl2 Bi1 Cl1 86.43(9) 2 2_554 ? 
Bi1 Cl1 Bi1 95.31(15) . 2 ? 
Bi1 Cl2 Bi1 97.62(11) . 2_554 ? 
C6 N1 C2 120.7(11) . . ? 
C3 C2 N1 114.0(12) . . ? 
C4 C3 C2 122.7(12) . . ? 
C5 C4 C3 122.3(13) . . ? 
C6 C5 C4 115.0(13) . . ? 
C5 C6 N1 123.8(12) . . ? 
 
_diffrn_measured_fraction_theta_max    0.972 
_diffrn_reflns_theta_full              25.19 
_diffrn_measured_fraction_theta_full   0.972 
_refine_diff_density_max    1.106 
_refine_diff_density_min   -1.015 
_refine_diff_density_rms    0.248 
