 
data_cohg12 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C7 H0 Br7 Co Hg3 N4 O3' 
_chemical_formula_weight          1408.18 
 
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' 
 'Co'  'Co'   0.3494   0.9721 
 '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                    7.431(9) 
_cell_length_b                    13.694(19) 
_cell_length_c                    13.722(15) 
_cell_angle_alpha                 68.68(6) 
_cell_angle_beta                  82.40(7) 
_cell_angle_gamma                 75.74(10) 
_cell_volume                      1259(3) 
_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     3.714 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1212 
_exptl_absorpt_coefficient_mu     29.995 
_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             4434 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.1184 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          3.04 
_diffrn_reflns_theta_max          25.15 
_reflns_number_total              4434 
_reflns_number_gt                 2529 
_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^)+(0.1000P)^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          4434 
_refine_ls_number_parameters      156 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.2321 
_refine_ls_R_factor_gt            0.1421 
_refine_ls_wR_factor_ref          0.3272 
_refine_ls_wR_factor_gt           0.2940 
_refine_ls_goodness_of_fit_ref    1.574 
_refine_ls_restrained_S_all       1.574 
_refine_ls_shift/su_max           1.025 
_refine_ls_shift/su_mean          0.175 
 
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 0.0453(3) 0.11147(14) 0.06670(13) 0.0398(6) Uani 1 d . . . 
Hg2 Hg 0.1944(3) 0.22906(17) 0.27841(16) 0.0552(7) Uani 1 d . . . 
Hg3 Hg -0.2724(3) 0.0510(2) 0.36776(19) 0.0714(8) Uani 1 d . . . 
Br1 Br -0.1558(7) 0.2412(4) 0.1389(3) 0.0428(12) Uani 1 d . . . 
Br2 Br 0.3935(7) 0.1104(4) 0.1806(4) 0.0459(12) Uani 1 d . . . 
Br3 Br -0.2535(7) 0.0232(4) -0.0057(4) 0.0476(12) Uani 1 d . . . 
Br4 Br -0.0886(7) -0.0727(4) 0.2870(4) 0.0511(13) Uani 1 d . . . 
Br5 Br 0.4911(8) 0.1624(6) 0.4445(5) 0.085(2) Uani 1 d . . . 
Br6 Br -0.0102(11) 0.1523(7) 0.4316(5) 0.104(3) Uani 1 d . . . 
Br7 Br 0.2040(8) 0.4242(5) 0.2018(5) 0.0671(16) Uani 1 d . . . 
Co Co 0.3293(7) 0.3109(4) -0.1890(4) 0.0243(12) Uani 1 d . . . 
N1 N 0.432(4) 0.175(2) -0.208(2) 0.016(6) Uiso 1 d . . . 
C1 C 0.594(5) 0.184(3) -0.290(3) 0.023(8) Uiso 1 d . . . 
C2 C 0.531(7) 0.298(4) -0.369(3) 0.046(12) Uiso 1 d . . . 
N2 N 0.499(4) 0.374(3) -0.303(2) 0.030(8) Uiso 1 d . . . 
C3 C 0.408(6) 0.482(3) -0.349(3) 0.039(11) Uiso 1 d . . . 
C4 C 0.355(7) 0.526(4) -0.262(4) 0.048(13) Uiso 1 d . . . 
N3 N 0.242(4) 0.458(2) -0.185(2) 0.023(7) Uiso 1 d . . . 
C5 C 0.277(7) 0.448(4) -0.070(3) 0.044(12) Uiso 1 d . . . 
C6 C 0.476(6) 0.384(4) -0.050(3) 0.042(12) Uiso 1 d . . . 
N4 N 0.496(4) 0.282(2) -0.076(2) 0.023(7) Uiso 1 d . . . 
O1 O 0.124(4) 0.261(2) -0.101(2) 0.042(8) Uiso 1 d . . . 
O2 O 0.115(4) 0.335(2) -0.269(2) 0.036(7) Uiso 1 d . . . 
C7 C 0.022(7) 0.294(4) -0.182(4) 0.043(13) Uiso 1 d . . . 
O3 O -0.140(4) 0.290(2) -0.181(2) 0.035(7) Uiso 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 0.0488(12) 0.0371(11) 0.0396(10) -0.0179(8) -0.0011(8) -0.0130(9) 
Hg2 0.0671(15) 0.0528(13) 0.0539(12) -0.0200(10) -0.0036(10) -0.0249(11) 
Hg3 0.0647(16) 0.0869(18) 0.0855(17) -0.0596(15) 0.0144(13) -0.0207(13) 
Br1 0.051(3) 0.043(3) 0.045(3) -0.025(2) -0.009(2) -0.011(2) 
Br2 0.041(3) 0.058(3) 0.048(3) -0.026(2) -0.011(2) -0.012(2) 
Br3 0.048(3) 0.053(3) 0.052(3) -0.026(2) -0.007(2) -0.013(2) 
Br4 0.052(3) 0.069(4) 0.044(3) -0.029(2) -0.002(2) -0.019(3) 
Br5 0.052(4) 0.143(6) 0.094(5) -0.090(5) -0.025(3) 0.005(4) 
Br6 0.113(6) 0.175(8) 0.051(3) -0.026(4) -0.001(4) -0.102(6) 
Br7 0.054(4) 0.060(4) 0.096(4) -0.029(3) -0.009(3) -0.023(3) 
Co 0.016(3) 0.033(3) 0.025(3) -0.006(2) -0.005(2) -0.011(2) 
 
_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 Br3 2.422(6) 2 ? 
Hg1 Br1 2.440(5) . ? 
Hg1 O1 2.58(3) . ? 
Hg2 Br6 2.484(7) . ? 
Hg2 Br7 2.507(7) . ? 
Hg2 Br2 2.551(6) . ? 
Hg2 Br5 3.117(7) . ? 
Hg3 Br4 2.406(6) . ? 
Hg3 Br5 2.426(6) 1_455 ? 
Hg3 Br6 3.027(8) . ? 
Br3 Hg1 2.422(6) 2 ? 
Br5 Hg3 2.426(6) 1_655 ? 
Co O1 1.92(3) . ? 
Co O2 1.95(3) . ? 
Co N4 1.98(3) . ? 
Co N1 1.93(3) . ? 
Co N2 1.95(3) . ? 
Co N3 1.98(3) . ? 
Co C7 2.34(5) . ? 
N1 C1 1.53(4) . ? 
C1 C2 1.54(6) . ? 
C2 N2 1.57(5) . ? 
N2 C3 1.42(5) . ? 
C3 C4 1.49(6) . ? 
C4 N3 1.46(6) . ? 
N3 C5 1.59(5) . ? 
C5 C6 1.52(6) . ? 
C6 N4 1.53(5) . ? 
O1 C7 1.30(6) . ? 
O2 C7 1.30(5) . ? 
C7 O3 1.21(5) . ? 
 
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 
Br3 Hg1 Br1 176.38(18) 2 . ? 
Br3 Hg1 O1 90.2(6) 2 . ? 
Br1 Hg1 O1 92.3(6) . . ? 
Br6 Hg2 Br7 123.9(3) . . ? 
Br6 Hg2 Br2 120.2(3) . . ? 
Br7 Hg2 Br2 115.8(2) . . ? 
Br6 Hg2 Br5 84.4(2) . . ? 
Br7 Hg2 Br5 97.1(2) . . ? 
Br2 Hg2 Br5 92.71(19) . . ? 
Br4 Hg3 Br5 168.6(2) . 1_455 ? 
Br4 Hg3 Br6 107.9(2) . . ? 
Br5 Hg3 Br6 83.5(3) 1_455 . ? 
Hg3 Br5 Hg2 97.2(2) 1_655 . ? 
Hg2 Br6 Hg3 109.5(2) . . ? 
O1 Co O2 67.8(12) . . ? 
O1 Co N4 97.6(13) . . ? 
O2 Co N4 164.7(11) . . ? 
O1 Co N1 93.0(12) . . ? 
O2 Co N1 91.1(12) . . ? 
N4 Co N1 94.1(12) . . ? 
O1 Co N2 167.2(14) . . ? 
O2 Co N2 99.5(13) . . ? 
N4 Co N2 95.0(13) . . ? 
N1 Co N2 88.1(12) . . ? 
O1 Co N3 93.3(12) . . ? 
O2 Co N3 89.0(12) . . ? 
N4 Co N3 87.5(13) . . ? 
N1 Co N3 173.2(11) . . ? 
N2 Co N3 85.2(12) . . ? 
O1 Co C7 33.9(13) . . ? 
O2 Co C7 33.9(13) . . ? 
N4 Co C7 131.2(14) . . ? 
N1 Co C7 93.5(15) . . ? 
N2 Co C7 133.4(15) . . ? 
N3 Co C7 90.4(15) . . ? 
C1 N1 Co 111(2) . . ? 
N1 C1 C2 102(3) . . ? 
C1 C2 N2 105(3) . . ? 
C3 N2 C2 119(3) . . ? 
C3 N2 Co 105(2) . . ? 
C2 N2 Co 102(2) . . ? 
N2 C3 C4 106(4) . . ? 
N3 C4 C3 107(4) . . ? 
C4 N3 C5 110(3) . . ? 
C4 N3 Co 108(3) . . ? 
C5 N3 Co 105(2) . . ? 
C6 C5 N3 105(3) . . ? 
C5 C6 N4 108(4) . . ? 
C6 N4 Co 110(2) . . ? 
C7 O1 Co 91(3) . . ? 
C7 O1 Hg1 120(3) . . ? 
Co O1 Hg1 142.4(15) . . ? 
C7 O2 Co 90(3) . . ? 
O3 C7 O1 127(4) . . ? 
O3 C7 O2 122(4) . . ? 
O1 C7 O2 111(4) . . ? 
O3 C7 Co 177(4) . . ? 
O1 C7 Co 55(2) . . ? 
O2 C7 Co 56(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.982 
_diffrn_reflns_theta_full              25.15 
_diffrn_measured_fraction_theta_full   0.982 
_refine_diff_density_max    3.926 
_refine_diff_density_min   -4.194 
_refine_diff_density_rms    0.737 
