 
data_exp_9019
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C10 H13 Co O8' 
_chemical_formula_weight          320.13

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'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    7.8186(19)
_cell_length_b                    8.4237(14)
_cell_length_c                    9.8767(17)
_cell_angle_alpha                 68.312(16)
_cell_angle_beta                  81.997(18)
_cell_angle_gamma                 87.309(16)
_cell_volume                      598.6(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     775
_cell_measurement_theta_min       4.8580
_cell_measurement_theta_max       69.9270
 
_exptl_crystal_description        block
_exptl_crystal_colour             violet
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.765          
_exptl_crystal_F_000              324
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.120
_exptl_crystal_size_mid           0.110
_exptl_crystal_size_min           0.110
_exptl_absorpt_coefficient_mu     11.607
_shelx_estimated_absorpt_T_min    0.336
_shelx_estimated_absorpt_T_max    0.362
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.16788
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Xcalibur, Eos, Gemini'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             3443
_diffrn_reflns_av_unetI/netI      0.0965
_diffrn_reflns_av_R_equivalents   0.0505
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          4.861
_diffrn_reflns_theta_max          67.243
_diffrn_reflns_theta_full         67.243
_diffrn_measured_fraction_theta_max   0.987
_diffrn_measured_fraction_theta_full  0.987
_diffrn_reflns_Laue_measured_fraction_max    0.987
_diffrn_reflns_Laue_measured_fraction_full   0.987
_diffrn_reflns_point_group_measured_fraction_max   0.987
_diffrn_reflns_point_group_measured_fraction_full  0.987
_reflns_number_total              2119
_reflns_number_gt                 1312
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1044P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2119
_refine_ls_number_parameters      172
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1100
_refine_ls_R_factor_gt            0.0696
_refine_ls_wR_factor_ref          0.1955
_refine_ls_wR_factor_gt           0.1690
_refine_ls_goodness_of_fit_ref    0.962
_refine_ls_restrained_S_all       0.962
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Co1 Co 0.52816(16) 1.15912(13) 0.11461(10) 0.0402(4) Uani 1 1 d . . . . .
O1 O 0.7480(7) 0.9810(6) 0.1436(5) 0.0519(14) Uani 1 1 d . . . . .
H1C H 0.794128 0.980844 0.060474 0.062 Uiso 1 1 d R U . . .
H1B H 0.709728 0.881914 0.198165 0.062 Uiso 1 1 d R U . . .
O2 O 0.3158(7) 1.3253(6) 0.0867(6) 0.0552(14) Uani 1 1 d . . . . .
H2B H 0.371977 1.418890 0.049741 0.066 Uiso 1 1 d R U . . .
H2A H 0.220097 1.363040 0.056041 0.066 Uiso 1 1 d R U . . .
O3 O 0.3606(7) 0.9690(6) 0.1545(5) 0.0454(13) Uani 1 1 d . . . . .
O4 O 0.3835(8) 0.7373(6) 0.1003(5) 0.0541(16) Uani 1 1 d . . . . .
O5 O 0.4542(7) 0.8531(6) 0.6759(4) 0.0419(12) Uani 1 1 d . . . . .
O6 O 0.3232(7) 0.6346(6) 0.8516(5) 0.0478(13) Uani 1 1 d . . . . .
O7 O 0.1687(6) 0.2633(5) 0.5838(5) 0.0429(12) Uani 1 1 d . . . . .
O8 O 1.0163(9) 0.2426(11) 0.0123(9) 0.110(3) Uani 1 1 d . . . . .
H8C H 0.927739 0.279724 0.051681 0.132 Uiso 1 1 d R U . . .
H8B H 1.011049 0.134504 0.039761 0.132 Uiso 1 1 d R U . . .
C1 C 0.3584(9) 0.8114(8) 0.1905(7) 0.0376(17) Uani 1 1 d . . . . .
C2 C 0.3230(9) 0.6980(8) 0.3483(7) 0.0331(15) Uani 1 1 d . . . . .
C3 C 0.3575(9) 0.7574(8) 0.4558(6) 0.0338(15) Uani 1 1 d . . . . .
H3 H 0.399755 0.867573 0.429393 0.041 Uiso 1 1 calc R U . . .
C4 C 0.2614(9) 0.5321(8) 0.3882(7) 0.0376(16) Uani 1 1 d . . . . .
H4 H 0.242020 0.491424 0.315936 0.045 Uiso 1 1 calc R U . . .
C5 C 0.2292(9) 0.4279(7) 0.5348(7) 0.0344(15) Uani 1 1 d . . . . .
C6 C 0.2627(9) 0.4886(8) 0.6420(6) 0.0362(16) Uani 1 1 d . . . . .
H6 H 0.240667 0.419179 0.740834 0.043 Uiso 1 1 calc R U . . .
C7 C 0.3285(9) 0.6515(8) 0.6023(7) 0.0335(15) Uani 1 1 d . . . . .
C8 C 0.3720(10) 0.7153(8) 0.7171(7) 0.0375(16) Uani 1 1 d . . . . .
C9 C 0.1184(10) 0.2050(8) 0.4758(7) 0.0411(17) Uani 1 1 d . . . . .
H9A H 0.218985 0.196774 0.409104 0.049 Uiso 1 1 calc R U . . .
H9B H 0.038083 0.284747 0.419035 0.049 Uiso 1 1 calc R U . . .
C10 C 0.0340(10) 0.0314(8) 0.5549(7) 0.0406(17) Uani 1 1 d . . . . .
H10A H -0.060866 0.038756 0.626969 0.049 Uiso 1 1 calc R U . . .
H10B H 0.117227 -0.049417 0.606439 0.049 Uiso 1 1 calc R U . . .
 
 
_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 O3 2.005(4) . ?
Co1 O4 2.006(4) 2_675 ?
Co1 O5 2.058(4) 2_676 ?
Co1 O2 2.101(6) . ?
Co1 O1 2.206(6) . ?
Co1 O6 2.282(5) 2_676 ?
Co1 C8 2.496(7) 2_676 ?
O3 C1 1.242(8) . ?
O4 C1 1.253(8) . ?
O5 C8 1.255(7) . ?
O6 C8 1.260(7) . ?
O7 C5 1.371(7) . ?
O7 C9 1.434(7) . ?
C1 C2 1.491(8) . ?
C2 C3 1.391(9) . ?
C2 C4 1.395(8) . ?
C3 C7 1.383(8) . ?
C4 C5 1.382(8) . ?
C5 C6 1.394(9) . ?
C6 C7 1.384(8) . ?
C7 C8 1.505(9) . ?
C9 C10 1.512(8) . ?
C10 C10 1.533(12) 2_556 ?
 
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
O3 Co1 O4 110.9(2) . 2_675 ?
O3 Co1 O5 101.39(18) . 2_676 ?
O4 Co1 O5 147.5(2) 2_675 2_676 ?
O3 Co1 O2 87.4(2) . . ?
O4 Co1 O2 91.2(2) 2_675 . ?
O5 Co1 O2 94.4(2) 2_676 . ?
O3 Co1 O1 91.5(2) . . ?
O4 Co1 O1 89.0(2) 2_675 . ?
O5 Co1 O1 86.1(2) 2_676 . ?
O2 Co1 O1 178.93(19) . . ?
O3 Co1 O6 160.30(18) . 2_676 ?
O4 Co1 O6 88.17(18) 2_675 2_676 ?
O5 Co1 O6 60.16(16) 2_676 2_676 ?
O2 Co1 O6 87.3(2) . 2_676 ?
O1 Co1 O6 93.78(19) . 2_676 ?
O3 Co1 C8 130.9(2) . 2_676 ?
O4 Co1 C8 118.2(2) 2_675 2_676 ?
O5 Co1 C8 30.06(18) 2_676 2_676 ?
O2 Co1 C8 89.6(2) . 2_676 ?
O1 Co1 C8 91.2(2) . 2_676 ?
O6 Co1 C8 30.15(18) 2_676 2_676 ?
C1 O3 Co1 139.8(5) . . ?
C1 O4 Co1 127.4(4) . 2_675 ?
C8 O5 Co1 94.7(4) . 2_676 ?
C8 O6 Co1 84.4(4) . 2_676 ?
C5 O7 C9 116.9(5) . . ?
O3 C1 O4 123.7(6) . . ?
O3 C1 C2 120.4(6) . . ?
O4 C1 C2 115.9(6) . . ?
C3 C2 C4 120.1(6) . . ?
C3 C2 C1 119.3(5) . . ?
C4 C2 C1 120.6(6) . . ?
C7 C3 C2 119.6(6) . . ?
C5 C4 C2 120.2(6) . . ?
O7 C5 C4 124.1(6) . . ?
O7 C5 C6 116.4(5) . . ?
C4 C5 C6 119.5(5) . . ?
C7 C6 C5 120.4(5) . . ?
C3 C7 C6 120.3(6) . . ?
C3 C7 C8 119.0(6) . . ?
C6 C7 C8 120.7(5) . . ?
O5 C8 O6 120.6(6) . . ?
O5 C8 C7 118.6(5) . . ?
O6 C8 C7 120.9(6) . . ?
O5 C8 Co1 55.2(3) . 2_676 ?
O6 C8 Co1 65.5(3) . 2_676 ?
C7 C8 Co1 173.3(5) . 2_676 ?
O7 C9 C10 108.2(5) . . ?
C9 C10 C10 110.3(7) . 2_556 ?
 
_refine_diff_density_max    0.772
_refine_diff_density_min   -0.865
_refine_diff_density_rms    0.116



