 
data_cuhg02 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C4 H0 Br4 Cu Hg N4 O0' 
_chemical_formula_weight          687.85 
 
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+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    8.055(3) 
_cell_length_b                    13.101(3) 
_cell_length_c                    13.814(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.24(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      1457.4(7) 
_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     3.135 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1204 
_exptl_absorpt_coefficient_mu     22.918 
_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      0.71069 
_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             5399 
_diffrn_reflns_av_R_equivalents   0.0884 
_diffrn_reflns_av_sigmaI/netI     0.0914 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          3.11 
_diffrn_reflns_theta_max          24.96 
_reflns_number_total              2563 
_reflns_number_gt                 1797 
_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^)+(0.0319P)^2^+13.5267P] 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          2563 
_refine_ls_number_parameters      130 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0928 
_refine_ls_R_factor_gt            0.0544 
_refine_ls_wR_factor_ref          0.1344 
_refine_ls_wR_factor_gt           0.1152 
_refine_ls_goodness_of_fit_ref    1.167 
_refine_ls_restrained_S_all       1.167 
_refine_ls_shift/su_max           0.013 
_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 
Hg1 Hg -0.22461(8) 0.19500(6) 0.24639(4) 0.0455(2) Uani 1 d . . . 
Br1 Br -0.1859(2) 0.19791(14) 0.06080(11) 0.0497(4) Uani 1 d . . . 
Br2 Br 0.0206(2) 0.28646(15) 0.33160(13) 0.0534(5) Uani 1 d . . . 
Br3 Br -0.1881(2) -0.00146(13) 0.30302(12) 0.0514(5) Uani 1 d . . . 
Br4 Br -0.5209(2) 0.23550(14) 0.29611(15) 0.0539(5) Uani 1 d . . . 
Cu1 Cu 0.5000 0.5000 0.5000 0.0379(6) Uani 1 d S . . 
N11 N 0.3797(17) 0.4833(10) 0.3725(9) 0.041(3) Uani 1 d . . . 
C11 C 0.236(4) 0.552(2) 0.3673(17) 0.107(11) Uani 1 d . . . 
C12 C 0.181(3) 0.582(2) 0.4571(15) 0.090(9) Uani 1 d . . . 
N12 N 0.6915(16) 0.4100(12) 0.4634(12) 0.057(4) Uani 1 d . . . 
Cu2 Cu 0.5000 0.5000 0.0000 0.0416(7) Uani 1 d S . . 
N21 N 0.4045(18) 0.3642(11) 0.0401(10) 0.050(4) Uani 1 d . . . 
C21 C 0.226(3) 0.3719(16) 0.0615(18) 0.078(7) Uani 1 d . . . 
C22 C 0.197(3) 0.475(2) 0.1067(19) 0.086(7) Uani 1 d . . . 
N22 N 0.2915(17) 0.5577(11) 0.0532(11) 0.048(4) Uani 1 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 
Hg1 0.0404(4) 0.0604(4) 0.0356(3) -0.0036(3) 0.0024(3) 0.0065(4) 
Br1 0.0674(11) 0.0517(10) 0.0300(8) -0.0023(8) 0.0040(7) 0.0136(10) 
Br2 0.0393(9) 0.0669(12) 0.0535(10) 0.0043(9) -0.0060(8) -0.0047(9) 
Br3 0.0681(11) 0.0444(10) 0.0418(9) 0.0029(8) 0.0052(8) 0.0114(9) 
Br4 0.0390(9) 0.0435(9) 0.0801(13) -0.0176(9) 0.0195(9) -0.0023(8) 
Cu1 0.0422(15) 0.0424(16) 0.0291(13) -0.0041(12) 0.0010(12) 0.0094(13) 
N11 0.049(8) 0.041(8) 0.034(7) -0.002(6) 0.002(6) 0.006(7) 
C11 0.12(2) 0.14(2) 0.060(14) -0.034(16) -0.031(15) 0.07(2) 
C12 0.055(12) 0.15(2) 0.059(12) -0.046(15) -0.033(10) 0.048(15) 
N12 0.033(7) 0.052(9) 0.087(11) -0.022(9) -0.016(8) 0.014(7) 
Cu2 0.0425(15) 0.0327(15) 0.0499(16) -0.0023(13) 0.0078(13) -0.0051(13) 
N21 0.055(9) 0.037(8) 0.057(9) -0.010(7) 0.009(7) -0.008(7) 
C21 0.059(13) 0.055(13) 0.120(19) -0.005(13) 0.048(13) -0.018(11) 
C22 0.087(16) 0.084(16) 0.089(17) -0.002(15) 0.026(14) -0.009(15) 
N22 0.041(8) 0.040(8) 0.065(9) 0.004(7) 0.016(7) -0.006(7) 
 
_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 Br4 2.554(2) . ? 
Hg1 Br2 2.573(2) . ? 
Hg1 Br1 2.5895(17) . ? 
Hg1 Br3 2.7043(19) . ? 
Cu1 N11 2.003(13) 3_666 ? 
Cu1 N11 2.003(13) . ? 
Cu1 N12 2.014(13) 3_666 ? 
Cu1 N12 2.014(13) . ? 
N11 C11 1.47(3) . ? 
C11 C12 1.38(3) . ? 
C12 N12 1.49(2) 3_666 ? 
N12 C12 1.49(2) 3_666 ? 
Cu2 N22 1.997(14) . ? 
Cu2 N22 1.997(14) 3_665 ? 
Cu2 N21 2.021(14) . ? 
Cu2 N21 2.021(14) 3_665 ? 
N21 C21 1.48(2) . ? 
C21 C22 1.51(3) . ? 
C22 N22 1.53(3) . ? 
 
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 
Br4 Hg1 Br2 119.53(7) . . ? 
Br4 Hg1 Br1 113.35(7) . . ? 
Br2 Hg1 Br1 109.78(7) . . ? 
Br4 Hg1 Br3 102.50(7) . . ? 
Br2 Hg1 Br3 103.48(7) . . ? 
Br1 Hg1 Br3 106.60(6) . . ? 
N11 Cu1 N11 180.000(2) 3_666 . ? 
N11 Cu1 N12 94.3(6) 3_666 3_666 ? 
N11 Cu1 N12 85.7(6) . 3_666 ? 
N11 Cu1 N12 85.7(6) 3_666 . ? 
N11 Cu1 N12 94.3(6) . . ? 
N12 Cu1 N12 180.000(3) 3_666 . ? 
C11 N11 Cu1 110.0(12) . . ? 
C12 C11 N11 113.1(19) . . ? 
C11 C12 N12 117.2(18) . 3_666 ? 
C12 N12 Cu1 106.8(11) 3_666 . ? 
N22 Cu2 N22 180.0 . 3_665 ? 
N22 Cu2 N21 84.5(6) . . ? 
N22 Cu2 N21 95.5(6) 3_665 . ? 
N22 Cu2 N21 95.5(6) . 3_665 ? 
N22 Cu2 N21 84.5(6) 3_665 3_665 ? 
N21 Cu2 N21 180.000(2) . 3_665 ? 
C21 N21 Cu2 111.9(12) . . ? 
N21 C21 C22 107.8(18) . . ? 
C21 C22 N22 110.6(17) . . ? 
C22 N22 Cu2 109.9(12) . . ? 
 
_diffrn_measured_fraction_theta_max    0.952 
_diffrn_reflns_theta_full              24.96 
_diffrn_measured_fraction_theta_full   0.952 
_refine_diff_density_max    1.173 
_refine_diff_density_min   -1.321 
_refine_diff_density_rms    0.266 
