 
data_crhg07 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C4 H0 Cl8 Cr Hg3 N4 O2' 
_chemical_formula_weight          1073.45 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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                    8.664(6) 
_cell_length_b                    10.751(5) 
_cell_length_c                    12.568(6) 
_cell_angle_alpha                 94.57(5) 
_cell_angle_beta                  104.84(6) 
_cell_angle_gamma                 105.18(5) 
_cell_volume                      1078.5(10) 
_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     3.305 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              936 
_exptl_absorpt_coefficient_mu     22.770 
_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             3699 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.1130 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          3.40 
_diffrn_reflns_theta_max          25.06 
_reflns_number_total              3699 
_reflns_number_gt                 2134 
_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^)+(0.1884P)^2^+108.4134P] 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          3699 
_refine_ls_number_parameters      149 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.2068 
_refine_ls_R_factor_gt            0.1306 
_refine_ls_wR_factor_ref          0.3811 
_refine_ls_wR_factor_gt           0.3084 
_refine_ls_goodness_of_fit_ref    1.051 
_refine_ls_restrained_S_all       1.051 
_refine_ls_shift/su_max           0.144 
_refine_ls_shift/su_mean          0.016 
 
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 1.0162(3) 0.46897(19) 0.16973(17) 0.0641(7) Uani 1 d . . . 
Hg2 Hg 0.5188(3) 0.36506(19) 0.12489(19) 0.0682(7) Uani 1 d . . . 
Hg3 Hg 0.3575(3) 0.6160(2) 0.5491(2) 0.0758(8) Uani 1 d . . . 
Cl1 Cl 0.7839(15) 0.3172(11) 0.2834(9) 0.054(3) Uani 1 d . . . 
Cl2 Cl 0.3842(16) 0.4319(13) 0.2616(11) 0.064(3) Uani 1 d . . . 
Cl3 Cl 0.7073(14) 0.5491(12) 0.0832(11) 0.061(3) Uani 1 d . . . 
Cl4 Cl 1.1250(17) 0.6515(11) 0.3050(10) 0.065(3) Uani 1 d . . . 
Cl5 Cl 0.3849(18) 0.1394(11) 0.0489(13) 0.076(4) Uani 1 d . . . 
Cl6 Cl 0.508(2) 0.1694(13) 0.4542(14) 0.081(4) Uani 1 d . . . 
Cl7 Cl 0.932(2) 0.3069(15) 0.0187(12) 0.084(4) Uani 1 d . . . 
Cl8 Cl 0.779(2) 0.6043(13) 0.4975(12) 0.095(5) Uani 1 d . . . 
Cr1 Cr 0.1691(10) 0.0668(7) 0.6873(7) 0.059(2) Uani 1 d . . . 
N11 N -0.024(5) -0.104(4) 0.675(3) 0.051(9) Uiso 1 d . . . 
C11 C -0.089(8) -0.096(7) 0.773(5) 0.091(19) Uiso 1 d . . . 
C12 C -0.082(10) 0.032(8) 0.823(6) 0.11(2) Uiso 1 d . . . 
N12 N 0.094(4) 0.131(4) 0.815(3) 0.050(9) Uiso 1 d . . . 
N21 N 0.349(5) 0.003(4) 0.794(3) 0.068(11) Uiso 1 d . . . 
C21 C 0.517(6) 0.103(5) 0.796(4) 0.054(11) Uiso 1 d . . . 
C22 C 0.505(7) 0.233(6) 0.805(5) 0.078(16) Uiso 1 d . . . 
N22 N 0.365(6) 0.239(5) 0.707(4) 0.082(14) Uiso 1 d . . . 
O10 O 0.014(5) 0.131(4) 0.586(3) 0.084(11) Uiso 1 d . . . 
O20 O 0.224(4) -0.010(4) 0.562(3) 0.067(9) 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 0.0683(14) 0.0406(11) 0.0783(14) -0.0109(9) 0.0190(10) 0.0152(9) 
Hg2 0.0730(14) 0.0383(11) 0.0923(16) 0.0070(9) 0.0286(11) 0.0108(9) 
Hg3 0.1068(19) 0.0394(12) 0.0892(16) 0.0099(10) 0.0379(13) 0.0255(11) 
Cl1 0.065(7) 0.042(6) 0.060(7) 0.007(5) 0.020(6) 0.021(5) 
Cl2 0.054(7) 0.069(8) 0.084(8) 0.014(6) 0.034(6) 0.029(6) 
Cl3 0.043(6) 0.050(7) 0.090(9) 0.021(6) 0.016(6) 0.013(5) 
Cl4 0.082(9) 0.037(6) 0.065(7) -0.005(5) 0.008(6) 0.017(6) 
Cl5 0.087(9) 0.025(6) 0.105(10) 0.009(6) 0.013(8) 0.014(6) 
Cl6 0.103(11) 0.038(7) 0.118(12) 0.024(7) 0.062(9) 0.018(7) 
Cl7 0.093(10) 0.071(10) 0.080(9) -0.029(7) 0.036(8) 0.013(8) 
Cl8 0.151(15) 0.034(7) 0.077(9) 0.000(6) 0.013(9) 0.013(8) 
Cr1 0.071(5) 0.037(4) 0.081(5) 0.011(4) 0.024(4) 0.031(4) 
 
_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 Cl7 2.295(12) . ? 
Hg1 Cl4 2.304(11) . ? 
Hg1 Cl1 2.980(13) . ? 
Hg2 Cl5 2.394(12) . ? 
Hg2 Cl3 2.402(13) . ? 
Hg2 Cl2 2.470(13) . ? 
Hg2 Cl1 2.819(12) . ? 
Hg3 Cl8 2.304(14) 2_666 ? 
Hg3 Cl6 2.306(13) 2_666 ? 
Hg3 Cl1 2.827(12) 2_666 ? 
Cl1 Hg3 2.827(12) 2_666 ? 
Cl6 Hg3 2.306(13) 2_666 ? 
Cl8 Hg3 2.304(14) 2_666 ? 
Cr1 O10 1.91(4) . ? 
Cr1 O20 1.94(4) . ? 
Cr1 N12 2.02(4) . ? 
Cr1 N21 2.08(4) . ? 
Cr1 N22 2.11(5) . ? 
Cr1 N11 2.10(4) . ? 
N11 C11 1.49(7) . ? 
C11 C12 1.45(10) . ? 
C12 N12 1.65(9) . ? 
N21 C21 1.57(7) . ? 
C21 C22 1.42(7) . ? 
C22 N22 1.51(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 
Cl7 Hg1 Cl4 170.8(6) . . ? 
Cl7 Hg1 Cl1 93.2(5) . . ? 
Cl4 Hg1 Cl1 95.9(4) . . ? 
Cl5 Hg2 Cl3 137.8(5) . . ? 
Cl5 Hg2 Cl2 109.2(5) . . ? 
Cl3 Hg2 Cl2 111.8(5) . . ? 
Cl5 Hg2 Cl1 94.4(4) . . ? 
Cl3 Hg2 Cl1 91.2(4) . . ? 
Cl2 Hg2 Cl1 95.6(4) . . ? 
Cl8 Hg3 Cl6 164.6(6) 2_666 2_666 ? 
Cl8 Hg3 Cl1 100.0(5) 2_666 2_666 ? 
Cl6 Hg3 Cl1 93.2(4) 2_666 2_666 ? 
Hg2 Cl1 Hg3 88.4(3) . 2_666 ? 
Hg2 Cl1 Hg1 88.1(3) . . ? 
Hg3 Cl1 Hg1 134.3(4) 2_666 . ? 
O10 Cr1 O20 89.4(16) . . ? 
O10 Cr1 N12 90.2(16) . . ? 
O20 Cr1 N12 174.5(16) . . ? 
O10 Cr1 N21 176.7(18) . . ? 
O20 Cr1 N21 88.9(16) . . ? 
N12 Cr1 N21 91.7(16) . . ? 
O10 Cr1 N22 92.1(19) . . ? 
O20 Cr1 N22 91.3(18) . . ? 
N12 Cr1 N22 94.2(18) . . ? 
N21 Cr1 N22 85.0(19) . . ? 
O10 Cr1 N11 89.4(16) . . ? 
O20 Cr1 N11 90.7(15) . . ? 
N12 Cr1 N11 83.8(15) . . ? 
N21 Cr1 N11 93.5(16) . . ? 
N22 Cr1 N11 177.5(16) . . ? 
C11 N11 Cr1 110(3) . . ? 
C12 C11 N11 118(6) . . ? 
C11 C12 N12 105(6) . . ? 
C12 N12 Cr1 113(3) . . ? 
C21 N21 Cr1 103(3) . . ? 
C22 C21 N21 111(4) . . ? 
C21 C22 N22 108(5) . . ? 
C22 N22 Cr1 106(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.966 
_diffrn_reflns_theta_full              25.06 
_diffrn_measured_fraction_theta_full   0.966 
_refine_diff_density_max    3.711 
_refine_diff_density_min   -3.837 
_refine_diff_density_rms    0.589 
