 
data_s92 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C12 H28 Cl2 Co N2 O4' 
_chemical_formula_weight          394.19 
 
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' 
 'Co'  'Co'   0.3494   0.9721 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            tetragonal 
_symmetry_space_group_name_H-M    P-42(1)c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z' 
 'y, -x, -z' 
 '-y, x, -z' 
 '-x+1/2, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z+1/2' 
 '-y+1/2, -x+1/2, z+1/2' 
 'y+1/2, x+1/2, z+1/2' 
 
_cell_length_a                    14.0554(4) 
_cell_length_b                    14.0554(4) 
_cell_length_c                    9.59290(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1895.12(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     13408 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        needle 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.80 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.382 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              828 
_exptl_absorpt_coefficient_mu     1.201 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details 	  'SORTAV (R. H. Blessing, 1997)'
_exptl_absorpt_correction_T_min   0.4466 
_exptl_absorpt_correction_T_max   0.8404 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(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   'Kappa Nonius CCD' 
_diffrn_measurement_method        '/f and /w scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             12738 
_diffrn_reflns_av_R_equivalents   0.0397 
_diffrn_reflns_av_sigmaI/netI     0.0249 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          2.57 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              1867 
_reflns_number_gt                 1480 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Denzo (Z. Otwinowski & W. Minor, 1997)' 
_computing_cell_refinement        'Denzo (Z. Otwinowski & W. Minor, 1997)'  
_computing_data_reduction         'SORTAV (R. H. Blessing, 1997)'
_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
_refine_ls_weighting_details      'calc w=1/[σ²(Fo²)+(0.0331P)²+0.0988P] where P=(Fo²+2Fc²)/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      SHELXL 
_refine_ls_extinction_coef        0.0072(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.015(15) 
_refine_ls_number_reflns          1867 
_refine_ls_number_parameters      148 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0352 
_refine_ls_R_factor_gt            0.0239 
_refine_ls_wR_factor_ref          0.0610 
_refine_ls_wR_factor_gt           0.0577 
_refine_ls_goodness_of_fit_ref    1.043 
_refine_ls_restrained_S_all       1.043 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 
Co1 Co 0.0000 0.5000 0.07928(3) 0.01763(13) Uani 1 d S . . 
Cl1 Cl 0.09336(3) 0.59314(3) -0.05488(5) 0.02657(15) Uani 1 d . . . 
O1 O 0.26777(9) 0.33592(9) 0.27918(13) 0.0299(3) Uani 1 d . . . 
O2 O 0.14921(9) 0.22377(9) 0.25058(14) 0.0314(3) Uani 1 d . . . 
N1 N 0.08673(11) 0.41326(11) 0.19367(18) 0.0207(3) Uani 1 d . . . 
H1A H 0.1190(14) 0.4489(15) 0.246(2) 0.039(7) Uiso 1 d . . . 
H1B H 0.0534(15) 0.3801(14) 0.241(2) 0.037(7) Uiso 1 d . . . 
C1 C 0.14929(15) 0.35580(14) 0.1027(2) 0.0251(4) Uani 1 d . . . 
H2A H 0.1865(15) 0.3974(14) 0.0535(19) 0.028(6) Uiso 1 d . . . 
H2B H 0.1105(15) 0.3189(15) 0.045(2) 0.033(6) Uiso 1 d . . . 
C2 C 0.21116(13) 0.28656(13) 0.1825(2) 0.0253(4) Uani 1 d . . . 
H2 H 0.2532(12) 0.2514(12) 0.114(2) 0.021(5) Uiso 1 d . . . 
C3 C 0.36593(15) 0.31080(17) 0.2784(2) 0.0380(5) Uani 1 d . . . 
H3A H 0.3912(15) 0.3342(16) 0.187(2) 0.063(7) Uiso 1 d . . . 
H3B H 0.3702(15) 0.2422(16) 0.277(2) 0.041(6) Uiso 1 d . . . 
C4 C 0.41443(18) 0.3561(2) 0.3990(2) 0.0425(6) Uani 1 d . . . 
H4A H 0.4841(17) 0.3433(19) 0.4044(19) 0.055(7) Uiso 1 d . . . 
H4B H 0.390(2) 0.335(2) 0.488(3) 0.089(9) Uiso 1 d . . . 
H4C H 0.4145(18) 0.4268(19) 0.393(2) 0.068(9) Uiso 1 d . . . 
C5 C 0.19605(15) 0.14292(16) 0.3084(2) 0.0398(5) Uani 1 d . . . 
H5A H 0.2371(18) 0.1705(17) 0.392(2) 0.063(7) Uiso 1 d . . . 
H5B H 0.2396(17) 0.1105(16) 0.237(2) 0.051(7) Uiso 1 d . . . 
C6 C 0.1237(2) 0.0749(2) 0.3590(3) 0.0644(8) Uani 1 d . . . 
H6A H 0.1547 0.0201 0.3978 0.100(11) Uiso 1 calc R . . 
H6B H 0.0839 0.0556 0.2827 0.18(2) Uiso 1 calc R . . 
H6C H 0.0854 0.1049 0.4293 0.109(12) Uiso 1 calc R . . 
 
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 
Co1 0.0183(2) 0.0174(2) 0.0172(2) 0.000 0.000 0.00059(13) 
Cl1 0.0267(3) 0.0283(3) 0.0247(3) 0.00255(17) 0.00215(17) -0.00831(19) 
O1 0.0221(7) 0.0336(8) 0.0341(7) -0.0125(6) -0.0046(6) 0.0075(6) 
O2 0.0296(8) 0.0260(7) 0.0386(7) 0.0064(6) -0.0030(6) 0.0046(6) 
N1 0.0214(9) 0.0211(9) 0.0195(9) -0.0017(7) 0.0012(7) 0.0013(7) 
C1 0.0270(11) 0.0271(11) 0.0212(11) -0.0011(8) 0.0007(8) 0.0062(8) 
C2 0.0241(11) 0.0272(11) 0.0245(11) -0.0048(7) -0.0003(7) 0.0070(8) 
C3 0.0232(11) 0.0405(14) 0.0504(15) -0.0147(11) -0.0040(10) 0.0065(10) 
C4 0.0300(14) 0.0544(17) 0.0431(14) -0.0079(12) -0.0058(10) 0.0008(12) 
C5 0.0407(14) 0.0367(13) 0.0419(12) 0.0068(11) -0.0029(11) 0.0112(11) 
C6 0.072(2) 0.0448(16) 0.077(2) 0.0272(15) 0.0187(18) 0.0080(15) 
 
_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 
Co1 N1 2.0436(16) . ? 
Co1 N1 2.0436(16) 2_565 ? 
Co1 Cl1 2.2565(5) 2_565 ? 
Co1 Cl1 2.2565(5) . ? 
O1 C2 1.405(2) . ? 
O1 C3 1.424(2) . ? 
O2 C2 1.401(2) . ? 
O2 C5 1.426(2) . ? 
N1 C1 1.479(3) . ? 
N1 H1A 0.844(19) . ? 
N1 H1B 0.804(19) . ? 
C1 C2 1.513(3) . ? 
C1 H1A 0.92(2) . ? 
C1 H1B 0.93(2) . ? 
C2 H2 1.01(2) . ? 
C3 C4 1.486(3) . ? 
C3 H3A 1.00(2) . ? 
C3 H3B 0.97(2) . ? 
C4 H4A 1.00(2) . ? 
C4 H4B 0.97(3) . ? 
C4 H4C 1.00(3) . ? 
C5 C6 1.478(3) . ? 
C5 H5A 1.06(2) . ? 
C5 H5B 1.02(2) . ? 
C6 H6A 0.9600 . ? 
C6 H6B 0.9600 . ? 
C6 H6C 0.9600 . ? 
 
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 
N1 Co1 N1 115.05(9) . 2_565 ? 
N1 Co1 Cl1 107.88(5) . 2_565 ? 
N1 Co1 Cl1 107.79(5) 2_565 2_565 ? 
N1 Co1 Cl1 107.79(5) . . ? 
N1 Co1 Cl1 107.88(5) 2_565 . ? 
Cl1 Co1 Cl1 110.45(3) 2_565 . ? 
C2 O1 C3 115.02(14) . . ? 
C2 O2 C5 113.34(14) . . ? 
C1 N1 Co1 111.32(12) . . ? 
C1 N1 H1A 111.0(14) . . ? 
Co1 N1 H1A 106.8(15) . . ? 
C1 N1 H1B 111.5(15) . . ? 
Co1 N1 H1B 107.7(16) . . ? 
H1A N1 H1B 108(2) . . ? 
N1 C1 C2 113.21(16) . . ? 
N1 C1 H1A 107.2(12) . . ? 
C2 C1 H1A 110.1(13) . . ? 
N1 C1 H1B 107.8(13) . . ? 
C2 C1 H1B 106.1(13) . . ? 
H1A C1 H1B 113(2) . . ? 
O2 C2 O1 110.82(17) . . ? 
O2 C2 C1 106.49(15) . . ? 
O1 C2 C1 109.99(15) . . ? 
O2 C2 H2 110.9(9) . . ? 
O1 C2 H2 109.7(10) . . ? 
C1 C2 H2 108.9(12) . . ? 
O1 C3 C4 109.53(18) . . ? 
O1 C3 H3A 105.5(13) . . ? 
C4 C3 H3A 112.2(14) . . ? 
O1 C3 H3B 107.9(13) . . ? 
C4 C3 H3B 114.1(12) . . ? 
H3A C3 H3B 107.1(19) . . ? 
C3 C4 H4A 114.5(12) . . ? 
C3 C4 H4B 112.8(19) . . ? 
H4A C4 H4B 105(2) . . ? 
C3 C4 H4C 112.5(14) . . ? 
H4A C4 H4C 100(2) . . ? 
H4B C4 H4C 111(2) . . ? 
O2 C5 C6 109.0(2) . . ? 
O2 C5 H5A 104.6(13) . . ? 
C6 C5 H5A 111.4(13) . . ? 
O2 C5 H5B 111.8(12) . . ? 
C6 C5 H5B 110.1(14) . . ? 
H5A C5 H5B 109.8(17) . . ? 
C5 C6 H6A 109.5 . . ? 
C5 C6 H6B 109.5 . . ? 
H6A C6 H6B 109.5 . . ? 
C5 C6 H6C 109.5 . . ? 
H6A C6 H6C 109.5 . . ? 
H6B C6 H6C 109.5 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
N1 Co1 N1 C1 -177.88(15) 2_565 . . . ? 
Cl1 Co1 N1 C1 61.78(13) 2_565 . . . ? 
Cl1 Co1 N1 C1 -57.50(13) . . . . ? 
Co1 N1 C1 C2 -176.91(13) . . . . ? 
C5 O2 C2 O1 -72.0(2) . . . . ? 
C5 O2 C2 C1 168.41(16) . . . . ? 
C3 O1 C2 O2 110.60(18) . . . . ? 
C3 O1 C2 C1 -131.92(18) . . . . ? 
N1 C1 C2 O2 62.1(2) . . . . ? 
N1 C1 C2 O1 -58.0(2) . . . . ? 
C2 O1 C3 C4 -171.07(19) . . . . ? 
C2 O2 C5 C6 -171.8(2) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              26.00 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.208 
_refine_diff_density_min   -0.276 
_refine_diff_density_rms    0.043 
