 
data_exp_10623 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C11.50 H14 Co O7' 
_chemical_formula_weight          323.16 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 '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' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Co'  'Co'  -2.3653   3.6143 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            triclinic 
_symmetry_space_group_name_H-M    P-1 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    7.6366(15) 
_cell_length_b                    8.6040(13) 
_cell_length_c                    10.0667(16) 
_cell_angle_alpha                 113.496(15) 
_cell_angle_beta                  90.956(15) 
_cell_angle_gamma                 90.157(14) 
_cell_volume                      606.47(18) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     666
_cell_measurement_theta_min       4.7830
_cell_measurement_theta_max       69.8530 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             red 
_exptl_crystal_size_max           0.12 
_exptl_crystal_size_mid           0.11 
_exptl_crystal_size_min           0.11 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.770 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              332 
_exptl_absorpt_coefficient_mu     11.401 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.3416 
_exptl_absorpt_correction_T_max   0.3669 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      1.54184 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Xcalibur, Eos, Gemini' 
_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             3600 
_diffrn_reflns_av_R_equivalents   0.0552 
_diffrn_reflns_av_sigmaI/netI     0.1020 
_diffrn_reflns_limit_h_min        -5 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          4.79 
_diffrn_reflns_theta_max          67.25 
_reflns_number_total              2143 
_reflns_number_gt                 1313 
_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  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1214P)²+0.0000P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2143 
_refine_ls_number_parameters      183 
_refine_ls_number_restraints      409 
_refine_ls_R_factor_all           0.1165 
_refine_ls_R_factor_gt            0.0661 
_refine_ls_wR_factor_ref          0.2003 
_refine_ls_wR_factor_gt           0.1605 
_refine_ls_goodness_of_fit_ref    0.909 
_refine_ls_restrained_S_all       0.836 
_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 
Co1 Co 0.46336(15) 0.33666(12) 0.09877(10) 0.0374(4) Uani 1 1 d U . . 
O1 O 0.6858(7) 0.1845(5) 0.0287(5) 0.0528(14) Uani 1 1 d U . . 
H1D H 0.6417 0.0691 -0.0040 0.063 Uiso 1 1 d R . . 
O2 O 0.2450(7) 0.5032(6) 0.1441(5) 0.0508(13) Uani 1 1 d U . . 
H2E H 0.3096 0.5852 0.1472 0.061 Uiso 1 1 d R . . 
O3 O 0.5373(6) 0.6458(5) 0.6845(5) 0.0402(11) Uani 1 1 d U . . 
O4 O 0.6710(6) 0.8608(5) 0.8498(4) 0.0394(11) Uani 1 1 d U . . 
O5 O 0.6277(6) 0.5379(5) 0.1573(4) 0.0413(11) Uani 1 1 d U . . 
O6 O 0.6092(6) 0.7705(5) 0.1131(4) 0.0403(11) Uani 1 1 d U . . 
O7 O 0.8319(6) 1.2330(5) 0.5886(4) 0.0383(11) Uani 1 1 d U . . 
C1 C 0.8407(12) 0.1853(9) 0.1036(8) 0.060(2) Uani 1 1 d U . . 
H1A H 0.8524 0.2908 0.1865 0.091 Uiso 1 1 calc R . . 
H1B H 0.9382 0.1722 0.0411 0.091 Uiso 1 1 calc R . . 
H1C H 0.8385 0.0935 0.1348 0.091 Uiso 1 1 calc R . . 
C3 C 0.6244(8) 0.7829(7) 0.7193(7) 0.0317(14) Uani 1 1 d U . . 
C4 C 0.6304(9) 0.6958(7) 0.1977(6) 0.0355(14) Uani 1 1 d U . . 
C5 C 0.6699(9) 0.8035(7) 0.3545(6) 0.0325(13) Uani 1 1 d U . . 
C6 C 0.6366(9) 0.7437(7) 0.4604(6) 0.0324(13) Uani 1 1 d U . . 
H6 H 0.5934 0.6340 0.4339 0.039 Uiso 1 1 calc R . . 
C7 C 0.6670(9) 0.8452(7) 0.6057(7) 0.0335(14) Uani 1 1 d U . . 
C8 C 0.7366(9) 1.0073(8) 0.6446(7) 0.0367(14) Uani 1 1 d U . . 
H8 H 0.7618 1.0748 0.7414 0.044 Uiso 1 1 calc R . . 
C9 C 0.7682(9) 1.0680(7) 0.5384(7) 0.0341(14) Uani 1 1 d U . . 
C10 C 0.7319(9) 0.9696(7) 0.3937(7) 0.0363(14) Uani 1 1 d U . . 
H10 H 0.7483 1.0131 0.3238 0.044 Uiso 1 1 calc R . . 
C11 C 0.8762(9) 1.2971(7) 0.4793(7) 0.0381(15) Uani 1 1 d U . . 
H11A H 0.7708 1.3115 0.4306 0.046 Uiso 1 1 calc R . . 
H11B H 0.9516 1.2179 0.4076 0.046 Uiso 1 1 calc R . . 
C12 C 0.9699(9) 1.4663(7) 0.5558(7) 0.0388(16) Uani 1 1 d U . . 
H12A H 1.0705 1.4524 0.6101 0.047 Uiso 1 1 calc R . . 
H12B H 0.8916 1.5467 0.6234 0.047 Uiso 1 1 calc R . . 
C2 C 0.094(2) 0.5120(19) 0.0783(17) 0.056(5) Uani 0.52(2) 1 d PU . . 
H2A H 0.0321 0.6118 0.1381 0.084 Uiso 0.50 1 calc PR . . 
H2B H 0.0233 0.4135 0.0631 0.084 Uiso 0.50 1 calc PR . . 
H2C H 0.1173 0.5168 -0.0133 0.084 Uiso 0.50 1 calc PR . . 
 
 
_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 O5 2.017(4) . ? 
Co1 O6 2.024(4) 2_665 ? 
Co1 O1 2.101(5) . ? 
Co1 O2 2.135(5) . ? 
Co1 O3 2.126(4) 2_666 ? 
Co1 O4 2.218(4) 2_666 ? 
O1 C1 1.391(9) . ? 
O2 C2 1.339(15) . ? 
O3 C3 1.270(7) . ? 
O3 Co1 2.126(4) 2_666 ? 
O4 C3 1.257(7) . ? 
O4 Co1 2.218(4) 2_666 ? 
O5 C4 1.254(7) . ? 
O6 C4 1.263(7) . ? 
O6 Co1 2.024(4) 2_665 ? 
O7 C9 1.387(7) . ? 
O7 C11 1.458(7) . ? 
C3 C7 1.483(8) . ? 
C4 C5 1.502(8) . ? 
C5 C6 1.383(8) . ? 
C5 C10 1.401(7) . ? 
C6 C7 1.388(8) . ? 
C7 C8 1.392(8) . ? 
C8 C9 1.388(9) . ? 
C9 C10 1.385(8) . ? 
C11 C12 1.518(8) . ? 
C12 C12 1.532(12) 2_786 ? 
 
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 
O5 Co1 O6 116.24(18) . 2_665 ? 
O5 Co1 O1 86.8(2) . . ? 
O6 Co1 O1 83.87(19) 2_665 . ? 
O5 Co1 O2 89.80(19) . . ? 
O6 Co1 O2 90.54(19) 2_665 . ? 
O1 Co1 O2 171.3(2) . . ? 
O5 Co1 O3 90.62(17) . 2_666 ? 
O6 Co1 O3 153.14(17) 2_665 2_666 ? 
O1 Co1 O3 98.1(2) . 2_666 ? 
O2 Co1 O3 89.91(19) . 2_666 ? 
O5 Co1 O4 149.94(17) . 2_666 ? 
O6 Co1 O4 93.33(16) 2_665 2_666 ? 
O1 Co1 O4 91.41(19) . 2_666 ? 
O2 Co1 O4 95.52(18) . 2_666 ? 
O3 Co1 O4 59.91(15) 2_666 2_666 ? 
C1 O1 Co1 129.6(4) . . ? 
C2 O2 Co1 137.0(8) . . ? 
C3 O3 Co1 92.8(4) . 2_666 ? 
C3 O4 Co1 89.0(3) . 2_666 ? 
C4 O5 Co1 142.5(5) . . ? 
C4 O6 Co1 126.8(4) . 2_665 ? 
C9 O7 C11 116.7(5) . . ? 
O4 C3 O3 118.3(5) . . ? 
O4 C3 C7 122.5(5) . . ? 
O3 C3 C7 119.2(5) . . ? 
O5 C4 O6 123.9(6) . . ? 
O5 C4 C5 118.4(5) . . ? 
O6 C4 C5 117.6(5) . . ? 
C6 C5 C10 119.9(6) . . ? 
C6 C5 C4 120.8(5) . . ? 
C10 C5 C4 119.2(5) . . ? 
C7 C6 C5 120.9(5) . . ? 
C6 C7 C8 119.4(6) . . ? 
C6 C7 C3 120.6(5) . . ? 
C8 C7 C3 120.0(6) . . ? 
C9 C8 C7 119.7(6) . . ? 
O7 C9 C8 115.3(5) . . ? 
O7 C9 C10 123.6(5) . . ? 
C8 C9 C10 121.1(5) . . ? 
C9 C10 C5 118.9(5) . . ? 
O7 C11 C12 107.7(5) . . ? 
C11 C12 C12 109.8(7) . 2_786 ? 
 
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              67.25 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    0.570 
_refine_diff_density_min   -0.528 
_refine_diff_density_rms    0.095 
