 
data_as3 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C4 H0 Br8 Cr Hg3 N4 O2' 
_chemical_formula_weight          1429.13 
 
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' 
 'Cr'  'Cr'   0.3209   0.6236 
 '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, -y, -z' 
 
_cell_length_a                    8.9103(10) 
_cell_length_b                    11.0101(11) 
_cell_length_c                    13.1896(17) 
_cell_angle_alpha                 94.905(14) 
_cell_angle_beta                  104.547(14) 
_cell_angle_gamma                 106.364(12) 
_cell_volume                      1184.6(2) 
_cell_formula_units_Z             2 
_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     4.007 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1224 
_exptl_absorpt_coefficient_mu     33.323 
_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             8155 
_diffrn_reflns_av_R_equivalents   0.0638 
_diffrn_reflns_av_sigmaI/netI     0.0851 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.32 
_diffrn_reflns_theta_max          26.02 
_reflns_number_total              4305 
_reflns_number_gt                 3008 
_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^)+(0.0601P)^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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4305 
_refine_ls_number_parameters      199 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0730 
_refine_ls_R_factor_gt            0.0474 
_refine_ls_wR_factor_ref          0.1121 
_refine_ls_wR_factor_gt           0.1038 
_refine_ls_goodness_of_fit_ref    0.927 
_refine_ls_restrained_S_all       0.927 
_refine_ls_shift/su_max           0.083 
_refine_ls_shift/su_mean          0.009 
 
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 -0.01278(7) 0.03281(6) 0.33164(5) 0.03515(18) Uani 1 d . . . 
Hg2 Hg -0.48023(8) -0.14047(6) 0.62719(6) 0.03872(18) Uani 1 d . . . 
Hg3 Hg -0.36301(9) -0.11876(6) 0.94170(6) 0.0453(2) Uani 1 d . . . 
Br1 Br -0.13726(18) -0.15976(13) 0.19587(12) 0.0324(4) Uani 1 d . . . 
Br2 Br 0.0704(2) 0.20653(17) 0.48169(15) 0.0502(5) Uani 1 d . . . 
Br3 Br -0.28829(19) 0.04573(15) 0.57627(15) 0.0411(4) Uani 1 d . . . 
Br4 Br -0.21113(19) -0.18386(14) 0.78363(13) 0.0360(4) Uani 1 d . . . 
Br5 Br -0.6277(2) -0.37377(14) 0.54673(13) 0.0354(4) Uani 1 d . . . 
Br6 Br -0.61699(17) -0.07058(14) 0.76443(13) 0.0326(4) Uani 1 d . . . 
Br7 Br -0.2110(3) 0.10787(15) 0.99867(14) 0.0512(5) Uani 1 d . . . 
Br8 Br -0.5089(2) -0.34149(15) 0.94967(16) 0.0437(4) Uani 1 d . . . 
Cr1 Cr -0.1662(3) 0.43307(19) 0.81444(17) 0.0203(5) Uani 1 d . . . 
N11 N -0.3479(13) 0.4841(10) 0.7114(10) 0.027(3) Uani 1 d . . . 
C11 C -0.5134(18) 0.3935(14) 0.7078(14) 0.037(4) Uani 1 d . . . 
C12 C -0.4980(18) 0.2593(14) 0.7029(12) 0.031(3) Uani 1 d . . . 
N12 N -0.3558(14) 0.2625(12) 0.7951(10) 0.031(3) Uani 1 d . . . 
N21 N -0.0901(13) 0.3660(10) 0.6884(9) 0.023(2) Uani 1 d . . . 
C21 C 0.065(3) 0.4572(19) 0.6908(19) 0.067(6) Uani 1 d . . . 
C22 C 0.076(3) 0.5907(19) 0.728(2) 0.084(9) Uani 1 d . . . 
N22 N 0.0182(14) 0.6020(10) 0.8193(10) 0.026(3) Uani 1 d . . . 
O10 O -0.0091(13) 0.3742(10) 0.9133(9) 0.039(3) Uani 1 d . . . 
O20 O -0.2154(12) 0.5124(10) 0.9375(8) 0.033(2) 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 2.4376(17) . ? 
Hg1 Br1 2.4413(16) . ? 
Hg1 Br4 3.0239(18) 2_556 ? 
Hg1 Br3 3.0445(16) 2_556 ? 
Hg2 Br5 2.5262(17) . ? 
Hg2 Br3 2.5330(18) . ? 
Hg2 Br6 2.5984(16) . ? 
Hg2 Br4 2.9263(17) . ? 
Hg3 Br7 2.4267(18) . ? 
Hg3 Br8 2.4559(18) . ? 
Hg3 Br4 2.8983(17) . ? 
Hg3 Br6 3.0166(17) . ? 
Br3 Hg1 3.0445(16) 2_556 ? 
Br4 Hg1 3.0239(18) 2_556 ? 
Cr1 O10 1.954(9) . ? 
Cr1 O20 1.979(9) . ? 
Cr1 N11 2.079(11) . ? 
Cr1 N12 2.088(13) . ? 
Cr1 N22 2.091(12) . ? 
Cr1 N21 2.099(11) . ? 
N11 C11 1.516(19) . ? 
C11 C12 1.519(19) . ? 
C12 N12 1.510(18) . ? 
N21 C21 1.45(2) . ? 
C21 C22 1.48(3) . ? 
C22 N22 1.43(2) . ? 
 
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 169.15(6) . . ? 
Br2 Hg1 Br4 94.00(6) . 2_556 ? 
Br1 Hg1 Br4 96.63(5) . 2_556 ? 
Br2 Hg1 Br3 91.08(6) . 2_556 ? 
Br1 Hg1 Br3 92.72(5) . 2_556 ? 
Br4 Hg1 Br3 81.08(5) 2_556 2_556 ? 
Br5 Hg2 Br3 135.08(6) . . ? 
Br5 Hg2 Br6 109.16(6) . . ? 
Br3 Hg2 Br6 113.70(6) . . ? 
Br5 Hg2 Br4 96.40(5) . . ? 
Br3 Hg2 Br4 92.24(5) . . ? 
Br6 Hg2 Br4 95.73(5) . . ? 
Br7 Hg3 Br8 160.17(7) . . ? 
Br7 Hg3 Br4 100.29(6) . . ? 
Br8 Hg3 Br4 95.62(6) . . ? 
Br7 Hg3 Br6 93.31(6) . . ? 
Br8 Hg3 Br6 99.11(6) . . ? 
Br4 Hg3 Br6 87.81(5) . . ? 
Hg2 Br3 Hg1 93.98(5) . 2_556 ? 
Hg3 Br4 Hg2 86.30(4) . . ? 
Hg3 Br4 Hg1 135.13(6) . 2_556 ? 
Hg2 Br4 Hg1 86.91(5) . 2_556 ? 
Hg2 Br6 Hg3 90.06(4) . . ? 
O10 Cr1 O20 88.9(4) . . ? 
O10 Cr1 N11 175.5(5) . . ? 
O20 Cr1 N11 90.0(4) . . ? 
O10 Cr1 N12 92.9(5) . . ? 
O20 Cr1 N12 92.7(5) . . ? 
N11 Cr1 N12 82.7(5) . . ? 
O10 Cr1 N22 90.3(5) . . ? 
O20 Cr1 N22 91.3(5) . . ? 
N11 Cr1 N22 94.1(4) . . ? 
N12 Cr1 N22 175.0(5) . . ? 
O10 Cr1 N21 89.6(4) . . ? 
O20 Cr1 N21 173.7(5) . . ? 
N11 Cr1 N21 92.0(4) . . ? 
N12 Cr1 N21 93.5(5) . . ? 
N22 Cr1 N21 82.6(4) . . ? 
C11 N11 Cr1 109.1(8) . . ? 
N11 C11 C12 106.8(11) . . ? 
N12 C12 C11 107.8(12) . . ? 
C12 N12 Cr1 109.2(9) . . ? 
C21 N21 Cr1 108.3(9) . . ? 
C22 C21 N21 112.1(14) . . ? 
N22 C22 C21 112.5(18) . . ? 
C22 N22 Cr1 109.6(10) . . ? 
 
_diffrn_measured_fraction_theta_max    0.925 
_diffrn_reflns_theta_full              26.02 
_diffrn_measured_fraction_theta_full   0.925 
_refine_diff_density_max    2.844 
_refine_diff_density_min   -2.244 
_refine_diff_density_rms    0.325 
