 
data_sb35pad 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum      'C20 H22 Co N2 O8' 
_chemical_formula_weight          477.33 
 
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' 
 'Co'  'Co'   0.3494   0.9721 
 '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' 
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    'C2/c'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    13.9240(13) 
_cell_length_b                    20.399(2) 
_cell_length_c                    9.2650(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  127.7460(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2080.9(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     273(2) 
_cell_measurement_reflns_used     5152 
_cell_measurement_theta_min       2.00 
_cell_measurement_theta_max       25.00 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.03 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.524 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              988 
_exptl_absorpt_coefficient_mu     0.875 
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.7817 
_exptl_absorpt_correction_T_max   0.9827 
_exptl_absorpt_process_details    'SADABS' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       273(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   'Bruker SMART APEX'
_diffrn_measurement_method        '\f and \w scans' 
_diffrn_detector_area_resol_mean  0 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5152 
_diffrn_reflns_av_R_equivalents   0.0452 
_diffrn_reflns_av_sigmaI/netI     0.0527 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -24 
_diffrn_reflns_limit_k_max        24 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        8 
_diffrn_reflns_theta_min          2.00 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              1829 
_reflns_number_gt                 1611 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0858P)^2^+3.9321P] 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          1829 
_refine_ls_number_parameters      141 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0739 
_refine_ls_R_factor_gt            0.0652 
_refine_ls_wR_factor_ref          0.1674 
_refine_ls_wR_factor_gt           0.1612 
_refine_ls_goodness_of_fit_ref    1.154 
_refine_ls_restrained_S_all       1.154 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Co Co 0.0000 0.24485(4) -0.2500 0.0223(3) Uani 1 2 d S . . 
O1 O 0.1266(3) 0.19619(15) -0.0215(4) 0.0349(8) Uani 1 1 d . . . 
O2 O -0.0284(3) 0.1404(2) -0.0761(6) 0.0691(13) Uani 1 1 d . . . 
O3 O 0.4021(3) 0.20401(14) 0.3033(4) 0.0293(7) Uani 1 1 d . . . 
O4 O 0.3645(3) 0.13353(16) 0.0908(4) 0.0360(8) Uani 1 1 d . . . 
C1 C 0.0834(4) 0.1486(2) 0.0130(7) 0.0345(11) Uani 1 1 d . . . 
C2 C 0.1696(4) 0.1034(2) 0.1646(6) 0.0306(10) Uani 1 1 d . . . 
C3 C 0.1224(5) 0.0558(3) 0.2148(8) 0.0489(14) Uani 1 1 d . . . 
H3 H 0.0389 0.0529 0.1511 0.059 Uiso 1 1 calc R . . 
C4 C 0.1976(6) 0.0136(3) 0.3564(9) 0.0608(17) Uani 1 1 d . . . 
H4 H 0.1647 -0.0183 0.3862 0.073 Uiso 1 1 calc R . . 
C5 C 0.3214(6) 0.0180(3) 0.4546(9) 0.0590(17) Uani 1 1 d . . . 
H5 H 0.3723 -0.0098 0.5531 0.071 Uiso 1 1 calc R . . 
C6 C 0.3698(5) 0.0642(2) 0.4059(7) 0.0397(12) Uani 1 1 d . . . 
H6 H 0.4535 0.0668 0.4714 0.048 Uiso 1 1 calc R . . 
C7 C 0.2954(4) 0.1066(2) 0.2611(6) 0.0271(10) Uani 1 1 d . . . 
C8 C 0.3562(4) 0.1517(2) 0.2103(6) 0.0253(9) Uani 1 1 d . . . 
C9 C 0.1707(5) 0.3156(3) 0.3076(8) 0.0485(14) Uani 1 1 d . . . 
H9A H 0.0853 0.3207 0.2061 0.058 Uiso 1 1 calc R . . 
H9B H 0.1967 0.3546 0.3828 0.058 Uiso 1 1 calc R . . 
C10 C 0.1864(6) 0.2569(3) 0.4191(8) 0.0568(16) Uani 1 1 d . . . 
H10A H 0.1377 0.2635 0.4603 0.068 Uiso 1 1 calc R . . 
H10B H 0.1547 0.2186 0.3406 0.068 Uiso 1 1 calc R . . 
N1 N 0.2410(4) 0.31010(19) 0.2356(5) 0.0340(9) Uani 1 1 d . . . 
H1A H 0.3077 0.3300 0.3058 0.041 Uiso 1 1 d R . . 
H1B H 0.2031 0.3266 0.1285 0.041 Uiso 1 1 d R . . 
H1C H 0.2546 0.2703 0.2307 0.041 Uiso 1 1 d 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 
Co 0.0190(5) 0.0270(5) 0.0259(5) 0.000 0.0162(4) 0.000 
O1 0.0311(19) 0.0343(17) 0.0352(18) 0.0102(14) 0.0182(16) 0.0060(14) 
O2 0.023(2) 0.083(3) 0.081(3) 0.022(2) 0.022(2) 0.0032(19) 
O3 0.0283(17) 0.0304(16) 0.0397(18) -0.0033(14) 0.0262(15) -0.0029(13) 
O4 0.0340(19) 0.0477(19) 0.0344(18) 0.0005(15) 0.0251(17) 0.0033(15) 
C1 0.029(3) 0.037(3) 0.038(3) 0.002(2) 0.020(2) 0.003(2) 
C2 0.031(3) 0.033(2) 0.037(3) 0.002(2) 0.026(2) 0.0003(19) 
C3 0.042(3) 0.051(3) 0.068(4) 0.008(3) 0.041(3) -0.007(3) 
C4 0.064(4) 0.052(3) 0.086(5) 0.028(3) 0.056(4) 0.002(3) 
C5 0.067(4) 0.048(3) 0.071(4) 0.031(3) 0.047(4) 0.015(3) 
C6 0.034(3) 0.039(3) 0.046(3) 0.012(2) 0.024(2) 0.008(2) 
C7 0.031(2) 0.027(2) 0.034(2) 0.0033(18) 0.025(2) 0.0018(18) 
C8 0.019(2) 0.032(2) 0.025(2) 0.0061(19) 0.0135(19) 0.0044(18) 
C9 0.052(3) 0.069(4) 0.053(3) 0.013(3) 0.047(3) 0.021(3) 
C10 0.049(4) 0.084(4) 0.055(4) 0.012(3) 0.041(3) 0.013(3) 
N1 0.035(2) 0.039(2) 0.035(2) 0.0029(17) 0.025(2) 0.0037(17) 
 
_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 
Co O1 2.002(3) . ? 
Co O1 2.002(3) 2_554 ? 
Co O3 2.004(3) 7 ? 
Co O3 2.004(3) 8_455 ? 
O1 C1 1.281(5) . ? 
O2 C1 1.249(6) . ? 
O3 C8 1.271(5) . ? 
O3 Co 2.004(3) 7 ? 
O4 C8 1.238(5) . ? 
C1 C2 1.483(6) . ? 
C2 C7 1.398(6) . ? 
C2 C3 1.401(6) . ? 
C3 C4 1.370(8) . ? 
C3 H3 0.9300 . ? 
C4 C5 1.373(8) . ? 
C4 H4 0.9300 . ? 
C5 C6 1.384(7) . ? 
C5 H5 0.9300 . ? 
C6 C7 1.386(6) . ? 
C6 H6 0.9300 . ? 
C7 C8 1.507(6) . ? 
C9 N1 1.488(5) . ? 
C9 C10 1.508(8) . ? 
C9 H9A 0.9700 . ? 
C9 H9B 0.9700 . ? 
C10 C10 1.488(12) 7_556 ? 
C10 H10A 0.9700 . ? 
C10 H10B 0.9700 . ? 
N1 H1A 0.8433 . ? 
N1 H1B 0.8574 . ? 
N1 H1C 0.8420 . ? 
 
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 
O1 Co O1 120.54(18) . 2_554 ? 
O1 Co O3 103.13(13) . 7 ? 
O1 Co O3 106.80(13) 2_554 7 ? 
O1 Co O3 106.80(13) . 8_455 ? 
O1 Co O3 103.13(13) 2_554 8_455 ? 
O3 Co O3 117.28(16) 7 8_455 ? 
C1 O1 Co 113.3(3) . . ? 
C8 O3 Co 113.9(3) . 7 ? 
O2 C1 O1 121.5(4) . . ? 
O2 C1 C2 120.0(4) . . ? 
O1 C1 C2 118.5(4) . . ? 
C7 C2 C3 118.6(4) . . ? 
C7 C2 C1 123.2(4) . . ? 
C3 C2 C1 118.3(4) . . ? 
C4 C3 C2 121.0(5) . . ? 
C4 C3 H3 119.5 . . ? 
C2 C3 H3 119.5 . . ? 
C3 C4 C5 120.4(5) . . ? 
C3 C4 H4 119.8 . . ? 
C5 C4 H4 119.8 . . ? 
C4 C5 C6 119.5(5) . . ? 
C4 C5 H5 120.3 . . ? 
C6 C5 H5 120.3 . . ? 
C5 C6 C7 121.1(5) . . ? 
C5 C6 H6 119.5 . . ? 
C7 C6 H6 119.5 . . ? 
C6 C7 C2 119.4(4) . . ? 
C6 C7 C8 116.9(4) . . ? 
C2 C7 C8 123.5(4) . . ? 
O4 C8 O3 125.0(4) . . ? 
O4 C8 C7 118.3(4) . . ? 
O3 C8 C7 116.5(4) . . ? 
N1 C9 C10 112.9(4) . . ? 
N1 C9 H9A 109.0 . . ? 
C10 C9 H9A 109.0 . . ? 
N1 C9 H9B 109.0 . . ? 
C10 C9 H9B 109.0 . . ? 
H9A C9 H9B 107.8 . . ? 
C10 C10 C9 115.1(7) 7_556 . ? 
C10 C10 H10A 108.5 7_556 . ? 
C9 C10 H10A 108.5 . . ? 
C10 C10 H10B 108.5 7_556 . ? 
C9 C10 H10B 108.5 . . ? 
H10A C10 H10B 107.5 . . ? 
C9 N1 H1A 109.5 . . ? 
C9 N1 H1B 112.5 . . ? 
H1A N1 H1B 108.1 . . ? 
C9 N1 H1C 109.2 . . ? 
H1A N1 H1C 109.1 . . ? 
H1B N1 H1C 108.4 . . ? 
 
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 
O1 Co O1 C1 -45.3(3) 2_554 . . . ? 
O3 Co O1 C1 -164.1(3) 7 . . . ? 
O3 Co O1 C1 71.7(3) 8_455 . . . ? 
Co O1 C1 O2 -8.9(6) . . . . ? 
Co O1 C1 C2 172.1(3) . . . . ? 
O2 C1 C2 C7 175.0(5) . . . . ? 
O1 C1 C2 C7 -5.9(7) . . . . ? 
O2 C1 C2 C3 -5.9(7) . . . . ? 
O1 C1 C2 C3 173.2(4) . . . . ? 
C7 C2 C3 C4 0.6(8) . . . . ? 
C1 C2 C3 C4 -178.6(5) . . . . ? 
C2 C3 C4 C5 1.3(10) . . . . ? 
C3 C4 C5 C6 -2.0(10) . . . . ? 
C4 C5 C6 C7 0.9(9) . . . . ? 
C5 C6 C7 C2 1.0(7) . . . . ? 
C5 C6 C7 C8 -175.6(5) . . . . ? 
C3 C2 C7 C6 -1.7(7) . . . . ? 
C1 C2 C7 C6 177.4(4) . . . . ? 
C3 C2 C7 C8 174.7(4) . . . . ? 
C1 C2 C7 C8 -6.2(7) . . . . ? 
Co O3 C8 O4 -3.0(5) 7 . . . ? 
Co O3 C8 C7 172.3(3) 7 . . . ? 
C6 C7 C8 O4 92.9(5) . . . . ? 
C2 C7 C8 O4 -83.6(5) . . . . ? 
C6 C7 C8 O3 -82.7(5) . . . . ? 
C2 C7 C8 O3 100.8(5) . . . . ? 
N1 C9 C10 C10 58.9(8) . . . 7_556 ? 
 
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    0.955 
_refine_diff_density_min   -0.784 
_refine_diff_density_rms    0.116 
