 
data_cuhg05 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C12 H0 Br4 Cu Hg N8 O4' 
_chemical_formula_weight          903.97 
 
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+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 
_cell_length_a                    8.2139(12) 
_cell_length_b                    12.6952(13) 
_cell_length_c                    24.106(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2513.7(5) 
_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     2.389 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1636 
_exptl_absorpt_coefficient_mu     13.336 
_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             5034 
_diffrn_reflns_av_R_equivalents   0.0421 
_diffrn_reflns_av_sigmaI/netI     0.0958 
_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        0 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.00 
_diffrn_reflns_theta_max          24.99 
_reflns_number_total              4392 
_reflns_number_gt                 2866 
_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^)+(0.0749P)^2^+81.3154P] 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    -0.05(3) 
_refine_ls_number_reflns          4392 
_refine_ls_number_parameters      261 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1548 
_refine_ls_R_factor_gt            0.0885 
_refine_ls_wR_factor_ref          0.2383 
_refine_ls_wR_factor_gt           0.1930 
_refine_ls_goodness_of_fit_ref    1.123 
_refine_ls_restrained_S_all       1.123 
_refine_ls_shift/su_max           0.009 
_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 0.14763(17) -0.09742(11) 0.19690(5) 0.0608(4) Uani 1 d . . . 
Br1 Br 0.2967(5) 0.0445(3) 0.25319(15) 0.0760(12) Uani 1 d . . . 
Br2 Br 0.1108(5) -0.0259(3) 0.09478(14) 0.0710(11) Uani 1 d . . . 
Br3 Br -0.1502(7) -0.1181(5) 0.22970(19) 0.1164(17) Uani 1 d . . . 
Br4 Br 0.2680(13) -0.2781(5) 0.1934(2) 0.222(5) Uani 1 d . . . 
Cu1 Cu -0.2552(4) -0.1038(3) 0.06314(12) 0.0439(8) Uani 1 d . . . 
O11 O -0.138(3) -0.1476(13) -0.0031(7) 0.044(4) Uani 1 d . . . 
C11 C -0.073(3) -0.235(2) 0.0003(12) 0.038(6) Uani 1 d . . . 
O12 O 0.006(3) -0.2748(15) -0.0407(8) 0.053(6) Uani 1 d . . . 
C12 C -0.076(4) -0.297(2) 0.0564(12) 0.050(7) Uiso 1 d . . . 
N11 N -0.183(3) -0.2401(16) 0.0952(10) 0.046(6) Uani 1 d . . . 
C13 C -0.157(4) -0.411(2) 0.0410(12) 0.060(8) Uani 1 d . . . 
C14 C -0.142(5) -0.494(2) 0.0886(11) 0.056(8) Uani 1 d . . . 
C15 C 0.031(4) -0.525(3) 0.0984(16) 0.075(11) Uani 1 d . . . 
N12 N 0.044(3) -0.615(2) 0.1374(9) 0.060(8) Uani 1 d . . . 
C16 C 0.055(3) -0.718(2) 0.1259(13) 0.046(7) Uani 1 d . . . 
N13 N 0.079(3) -0.784(2) 0.1667(11) 0.056(7) Uani 1 d . . . 
N14 N 0.055(4) -0.755(2) 0.0732(11) 0.072(9) Uani 1 d . . . 
O21 O -0.303(2) 0.0313(14) 0.0294(6) 0.040(5) Uani 1 d . . . 
C21 C -0.401(3) 0.088(2) 0.0567(10) 0.040(6) Uani 1 d . . . 
O22 O -0.472(3) 0.1670(16) 0.0369(8) 0.058(6) Uani 1 d . . . 
C22 C -0.441(3) 0.0597(18) 0.1182(10) 0.027(5) Uani 1 d . . . 
N21 N -0.404(3) -0.0584(16) 0.1239(10) 0.046(6) Uani 1 d . . . 
C23 C -0.334(3) 0.1204(16) 0.1553(9) 0.031(6) Uani 1 d . . . 
C24 C -0.344(4) 0.2424(19) 0.1528(10) 0.037(6) Uiso 1 d . . . 
C25 C -0.511(3) 0.2813(17) 0.1604(9) 0.029(6) Uani 1 d . . . 
N22 N -0.516(3) 0.3979(18) 0.1536(8) 0.040(5) Uani 1 d . . . 
C26 C -0.547(3) 0.443(2) 0.1081(10) 0.044(7) Uani 1 d . . . 
N23 N -0.573(3) 0.3852(18) 0.0611(10) 0.052(6) Uani 1 d . . . 
N24 N -0.566(3) 0.5508(17) 0.1061(8) 0.051(7) 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 Br4 2.499(5) . ? 
Hg1 Br1 2.566(4) . ? 
Hg1 Br3 2.584(6) . ? 
Hg1 Br2 2.641(4) . ? 
Cu1 O21 1.938(17) . ? 
Cu1 O11 1.947(18) . ? 
Cu1 N11 1.99(2) . ? 
Cu1 N21 1.99(2) . ? 
O11 C11 1.23(3) . ? 
C11 O12 1.29(3) . ? 
C11 C12 1.57(4) . ? 
C12 N11 1.48(4) . ? 
C12 C13 1.63(4) . ? 
C13 C14 1.57(4) . ? 
C14 C15 1.49(5) . ? 
C15 N12 1.48(4) . ? 
N12 C16 1.34(4) . ? 
C16 N13 1.31(4) . ? 
C16 N14 1.36(4) . ? 
O21 C21 1.26(3) . ? 
C21 O22 1.25(3) . ? 
C21 C22 1.56(3) . ? 
C22 C23 1.47(3) . ? 
C22 N21 1.54(3) . ? 
C23 C24 1.55(3) . ? 
C24 C25 1.47(4) . ? 
C25 N22 1.49(3) . ? 
N22 C26 1.26(3) . ? 
C26 N23 1.37(4) . ? 
C26 N24 1.37(4) . ? 
 
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 Br1 118.3(2) . . ? 
Br4 Hg1 Br3 107.0(3) . . ? 
Br1 Hg1 Br3 111.17(17) . . ? 
Br4 Hg1 Br2 109.20(16) . . ? 
Br1 Hg1 Br2 107.84(12) . . ? 
Br3 Hg1 Br2 102.23(14) . . ? 
O21 Cu1 O11 90.6(7) . . ? 
O21 Cu1 N11 174.2(9) . . ? 
O11 Cu1 N11 85.5(8) . . ? 
O21 Cu1 N21 85.8(8) . . ? 
O11 Cu1 N21 171.6(9) . . ? 
N11 Cu1 N21 98.6(9) . . ? 
C11 O11 Cu1 114.6(18) . . ? 
O11 C11 O12 121(3) . . ? 
O11 C11 C12 120(3) . . ? 
O12 C11 C12 118(2) . . ? 
N11 C12 C11 108(2) . . ? 
N11 C12 C13 109(2) . . ? 
C11 C12 C13 105(2) . . ? 
C12 N11 Cu1 111.1(18) . . ? 
C14 C13 C12 113(3) . . ? 
C15 C14 C13 112(3) . . ? 
N12 C15 C14 112(3) . . ? 
C16 N12 C15 129(3) . . ? 
N13 C16 N12 119(3) . . ? 
N13 C16 N14 119(3) . . ? 
N12 C16 N14 122(3) . . ? 
C21 O21 Cu1 114.8(16) . . ? 
O22 C21 O21 124(2) . . ? 
O22 C21 C22 117(2) . . ? 
O21 C21 C22 119(2) . . ? 
C23 C22 N21 110.0(18) . . ? 
C23 C22 C21 109.4(19) . . ? 
N21 C22 C21 106(2) . . ? 
C22 N21 Cu1 109.6(15) . . ? 
C22 C23 C24 118(2) . . ? 
C25 C24 C23 112(2) . . ? 
C24 C25 N22 110(2) . . ? 
C26 N22 C25 124(2) . . ? 
N22 C26 N23 120(3) . . ? 
N22 C26 N24 120(2) . . ? 
N23 C26 N24 119(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              24.99 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    1.549 
_refine_diff_density_min   -2.068 
_refine_diff_density_rms    0.276 
