 
data_as2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C12 H0 Br6 Cu Hg2 N4 O4' 
_chemical_formula_weight          1208.34 
 
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' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 'Cu'  'Cu'   0.3201   1.2651 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Hg'  'Hg'  -2.3894   9.2266 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y, z' 
 'x+1/2, y+1/2, z+1/2' 
 'x+1, -y+1/2, z+1/2' 
 
_cell_length_a                    15.0482(14) 
_cell_length_b                    9.2466(7) 
_cell_length_c                    21.508(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  110.134(11) 
_cell_angle_gamma                 90.00 
_cell_volume                      2809.9(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.856 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2124 
_exptl_absorpt_coefficient_mu     20.204 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5142 
_diffrn_reflns_av_R_equivalents   0.0553 
_diffrn_reflns_av_sigmaI/netI     0.0578 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          2.02 
_diffrn_reflns_theta_max          25.90 
_reflns_number_total              2718 
_reflns_number_gt                 2222 
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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^)+(0.0618P)^2^+100.8614P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.12(4) 
_refine_ls_number_reflns          2718 
_refine_ls_number_parameters      227 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0670 
_refine_ls_R_factor_gt            0.0539 
_refine_ls_wR_factor_ref          0.1497 
_refine_ls_wR_factor_gt           0.1415 
_refine_ls_goodness_of_fit_ref    1.134 
_refine_ls_restrained_S_all       1.133 
_refine_ls_shift/su_max           0.024 
_refine_ls_shift/su_mean          0.003 
 
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 
Hg1 Hg 0.99988(8) 0.13962(18) 0.99963(6) 0.0390(4) Uani 1 d . . . 
Hg2 Hg 1.02997(8) 0.35361(18) 0.84842(6) 0.0400(4) Uani 1 d . . . 
Br1 Br 0.8301(3) 0.0554(5) 0.96895(19) 0.0374(10) Uani 1 d . . . 
Br2 Br 1.1273(6) 0.1504(7) 1.1049(4) 0.096(3) Uani 1 d . . . 
Br3 Br 0.9728(4) 0.4342(4) 0.9505(2) 0.0429(11) Uani 1 d . . . 
Br4 Br 1.0616(3) 0.0688(4) 0.9015(2) 0.0398(10) Uani 1 d . . . 
Br5 Br 0.8893(5) 0.3394(8) 0.7411(3) 0.081(2) Uani 1 d . . . 
Br6 Br 1.2009(3) 0.4367(4) 0.8812(3) 0.0432(12) Uani 1 d . . . 
Cu1 Cu 1.0212(4) 0.7547(7) 0.9291(3) 0.0253(6) Uani 1 d . . . 
O11 O 1.016(2) 0.796(3) 1.0155(14) 0.034(7) Uiso 1 d . . . 
O12 O 1.082(2) 0.770(4) 1.1192(12) 0.042(8) Uani 1 d . . . 
C11 C 1.076(3) 0.762(4) 1.061(2) 0.029(8) Uani 1 d . . . 
C12 C 1.157(2) 0.675(3) 1.0435(13) 0.028(5) Uiso 1 d . . . 
N11 N 1.1513(18) 0.712(3) 0.9789(11) 0.017(5) Uani 1 d . . . 
C13 C 1.253(2) 0.711(4) 1.0913(16) 0.047(8) Uani 1 d . . . 
C14 C 1.328(3) 0.596(4) 1.0665(19) 0.039(8) Uiso 1 d . . . 
C15 C 1.320(4) 0.446(5) 1.088(2) 0.073(12) Uiso 1 d . . . 
C16 C 1.339(2) 0.328(3) 1.0667(11) 0.033(7) Uani 1 d . . . 
N12 N 1.3808(18) 0.201(4) 1.0923(13) 0.031(7) Uani 1 d . . . 
O21 O 1.0239(19) 0.703(3) 0.8419(12) 0.031(6) Uani 1 d . . . 
O22 O 0.939(2) 0.742(3) 0.7308(11) 0.039(8) Uani 1 d . . . 
C21 C 0.938(3) 0.747(4) 0.7915(15) 0.029(9) Uani 1 d . . . 
C22 C 0.856(2) 0.759(4) 0.8075(15) 0.041(7) Uiso 1 d . . . 
N21 N 0.878(3) 0.786(4) 0.8843(12) 0.049(11) Uani 1 d . . . 
C23 C 0.792(3) 0.893(4) 0.7675(17) 0.051(9) Uani 1 d . . . 
C24 C 0.693(2) 0.877(4) 0.7689(12) 0.032(7) Uani 1 d . . . 
C25 C 0.647(2) 1.035(3) 0.7456(13) 0.029(5) Uiso 1 d . . . 
C26 C 0.634(4) 1.109(6) 0.772(3) 0.082(14) Uiso 1 d . . . 
N22 N 0.635(3) 1.298(5) 0.7467(16) 0.055(11) Uani 1 d . . . 
 
 
_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 
Hg1 Br2 2.414(6) . ? 
Hg1 Br1 2.531(5) . ? 
Hg1 Br4 2.665(5) . ? 
Hg1 Br3 2.899(4) . ? 
Hg2 Br6 2.541(5) . ? 
Hg2 Br5 2.542(6) . ? 
Hg2 Br3 2.722(6) . ? 
Hg2 Br4 2.845(4) . ? 
Cu1 N11 1.92(3) . ? 
Cu1 O11 1.92(3) . ? 
Cu1 O21 1.95(3) . ? 
Cu1 N21 2.05(3) . ? 
O11 C11 1.12(5) . ? 
O12 C11 1.23(5) . ? 
C11 C12 1.61(4) . ? 
C12 N11 1.40(3) . ? 
C12 C13 1.49(4) . ? 
C13 C14 1.76(5) . ? 
C14 C15 1.48(6) . ? 
C15 C16 1.26(5) . ? 
C16 N12 1.35(5) . ? 
O21 C21 1.43(4) . ? 
O22 C21 1.31(4) . ? 
C21 C22 1.39(5) . ? 
C22 N21 1.59(4) . ? 
C22 C23 1.62(5) . ? 
C23 C24 1.51(5) . ? 
C24 C25 1.62(4) . ? 
C25 C26 0.95(5) . ? 
C26 N22 1.83(7) . ? 
 
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 
Br2 Hg1 Br1 131.4(3) . . ? 
Br2 Hg1 Br4 111.9(3) . . ? 
Br1 Hg1 Br4 108.29(15) . . ? 
Br2 Hg1 Br3 105.7(2) . . ? 
Br1 Hg1 Br3 101.04(16) . . ? 
Br4 Hg1 Br3 89.17(15) . . ? 
Br6 Hg2 Br5 135.6(2) . . ? 
Br6 Hg2 Br3 105.31(17) . . ? 
Br5 Hg2 Br3 110.5(2) . . ? 
Br6 Hg2 Br4 98.89(16) . . ? 
Br5 Hg2 Br4 106.8(2) . . ? 
Br3 Hg2 Br4 89.18(15) . . ? 
Hg2 Br3 Hg1 89.62(13) . . ? 
Hg1 Br4 Hg2 91.96(13) . . ? 
N11 Cu1 O11 82.8(11) . . ? 
N11 Cu1 O21 97.5(10) . . ? 
O11 Cu1 O21 177.3(17) . . ? 
N11 Cu1 N21 173.1(14) . . ? 
O11 Cu1 N21 92.4(13) . . ? 
O21 Cu1 N21 87.0(12) . . ? 
C11 O11 Cu1 120(3) . . ? 
O11 C11 O12 129(4) . . ? 
O11 C11 C12 113(3) . . ? 
O12 C11 C12 118(3) . . ? 
N11 C12 C13 110(2) . . ? 
N11 C12 C11 109(2) . . ? 
C13 C12 C11 111(3) . . ? 
C12 N11 Cu1 107.7(18) . . ? 
C12 C13 C14 103(3) . . ? 
C15 C14 C13 110(3) . . ? 
C16 C15 C14 130(4) . . ? 
C15 C16 N12 137(3) . . ? 
C21 O21 Cu1 110(2) . . ? 
O22 C21 C22 124(3) . . ? 
O22 C21 O21 115(4) . . ? 
C22 C21 O21 119(3) . . ? 
C21 C22 N21 112(3) . . ? 
C21 C22 C23 110(3) . . ? 
N21 C22 C23 108(2) . . ? 
C22 N21 Cu1 106(2) . . ? 
C24 C23 C22 109(2) . . ? 
C23 C24 C25 103(3) . . ? 
C26 C25 C24 128(4) . . ? 
C25 C26 N22 119(5) . . ? 
 
_diffrn_measured_fraction_theta_max    0.496 
_diffrn_reflns_theta_full              25.90 
_diffrn_measured_fraction_theta_full   0.496 
_refine_diff_density_max    1.386 
_refine_diff_density_min   -1.482 
_refine_diff_density_rms    0.278 
