 
data_r-3
 
_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
 'C5.56 H Co O4.56' 
_chemical_formula_weight          199.67

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'  -0.0020   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'
 'O'  'O'  -0.0041   0.0059
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.2027   0.9509
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            148
_space_group_name_H-M_alt         'R -3 :H'
_space_group_name_Hall            '-R 3'
 
_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'
 '-y, x-y, z'
 '-x+y, -x, z'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 '-x+y+2/3, -x+1/3, z+1/3'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 '-x+y+1/3, -x+2/3, z+2/3'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-x+2/3, -y+1/3, -z+1/3'
 'y+2/3, -x+y+1/3, -z+1/3'
 'x-y+2/3, x+1/3, -z+1/3'
 '-x+1/3, -y+2/3, -z+2/3'
 'y+1/3, -x+y+2/3, -z+2/3'
 'x-y+1/3, x+2/3, -z+2/3'
 
_cell_length_a                    25.844(4)
_cell_length_b                    25.844(4)
_cell_length_c                    6.8710(14)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      3974.5(14)
_cell_formula_units_Z             18
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     127237
_cell_measurement_theta_min       0.57
_cell_measurement_theta_max       50.00
 
_exptl_crystal_description        'hexagonal column'
_exptl_crystal_colour              purple
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.502          
_exptl_crystal_F_000              1761
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.110
_exptl_crystal_size_mid           0.040
_exptl_crystal_size_min           0.020
_exptl_absorpt_coefficient_mu     1.824
_shelx_estimated_absorpt_T_min    0.825
_shelx_estimated_absorpt_T_max    0.964
_exptl_absorpt_correction_type    'empirical'
_exptl_absorpt_correction_T_min   0.764
_exptl_absorpt_correction_T_max   1.294
_exptl_absorpt_process_details    'HKL3000sm Scalepack (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.700
_diffrn_radiation_type            synchrotron
_diffrn_source                    'PLSII 2D bending magnet'
_diffrn_measurement_device_type   'ADSC Q210 CCD area detector' 
_diffrn_measurement_method        'omega scan' 
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             4344
_diffrn_reflns_av_unetI/netI      0.0220
_diffrn_reflns_av_R_equivalents   ?
_diffrn_reflns_limit_h_min        -44
_diffrn_reflns_limit_h_max        43
_diffrn_reflns_limit_k_min        -44
_diffrn_reflns_limit_k_max        44
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          3.054
_diffrn_reflns_theta_max          37.625
_diffrn_reflns_theta_full         24.835
_diffrn_measured_fraction_theta_max   0.887
_diffrn_measured_fraction_theta_full  0.996
_diffrn_reflns_Laue_measured_fraction_max    0.887
_diffrn_reflns_Laue_measured_fraction_full   0.996
_diffrn_reflns_point_group_measured_fraction_max   0.887
_diffrn_reflns_point_group_measured_fraction_full  0.996
_reflns_number_total              4344
_reflns_number_gt                 3968
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
 
_computing_data_collection        'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction         'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-2018/3 (Sheldrick, 2018)' 
_computing_molecular_graphics     'DIAMOND 4 (Putz & Brandenburg, 2014)'
_computing_publication_material   'enCifer 1.5.1'
_refine_special_details
;
 Refined as a 4-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1416P)²+0.3723P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.045(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          4344
_refine_ls_number_parameters      115
_refine_ls_number_restraints      8
_refine_ls_R_factor_all           0.0636
_refine_ls_R_factor_gt            0.0604
_refine_ls_wR_factor_ref          0.1676
_refine_ls_wR_factor_gt           0.1629
_refine_ls_goodness_of_fit_ref    1.051
_refine_ls_restrained_S_all       1.052
_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 0.30016(2) 0.01857(2) 0.31395(3) 0.01671(11) Uani 1 1 d . . . . .
O1 O 0.35573(5) 0.08169(5) 0.50274(16) 0.0185(2) Uani 1 1 d . . . . .
O2 O 0.37082(5) 0.00981(5) 0.18822(17) 0.0186(2) Uani 1 1 d . . . . .
O3 O 0.30172(6) 0.07193(6) 0.09405(17) 0.0208(2) Uani 1 1 d . . . . .
C1 C 0.34401(7) 0.12169(7) 0.5875(2) 0.0183(2) Uani 1 1 d . . . . .
C2 C 0.34886(7) 0.16884(7) 0.4736(2) 0.0191(2) Uani 1 1 d . . . . .
H2 H 0.359347 0.170502 0.340322 0.023 Uiso 1 1 calc R U . . .
C3 C 0.33898(7) 0.21359(7) 0.5472(2) 0.0183(2) Uani 1 1 d . . . . .
C4 C 0.34941(7) 0.26306(7) 0.4120(2) 0.0184(2) Uani 1 1 d . . . . .
C1C C 0.22219(10) 0.01878(11) 0.4225(3) 0.0330(4) Uani 0.95 1 d . . P . .
O1C O 0.18214(15) 0.0213(2) 0.4610(5) 0.0818(11) Uani 0.95 1 d . . P . .
O2C O 0.4679(7) 0.1741(7) 0.1968(19) 0.194(6) Uani 0.61 1 d D U P . .
C2C C 0.4885(7) 0.1916(9) 0.345(3) 0.175(8) Uani 0.61 1 d D U P . .
 
 
_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 O1 2.0157(12) . ?
Co1 O1 2.0213(12) 8_544 ?
Co1 O3 2.0324(12) . ?
Co1 O2 2.0879(12) 6 ?
Co1 O2 2.1320(12) . ?
Co1 C1C 2.151(2) . ?
O1 C1 1.3463(19) . ?
O2 C4 1.2749(19) 18_545 ?
O3 C4 1.2604(19) 13 ?
C1 C2 1.400(2) . ?
C1 C3 1.422(2) 13_556 ?
C2 C3 1.398(2) . ?
C3 C4 1.492(2) . ?
C1C O1C 1.102(3) . ?
O2C C2C 1.134(15) . ?
 
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 Co1 O1 163.38(5) . 8_544 ?
O1 Co1 O3 99.50(5) . . ?
O1 Co1 O3 95.87(5) 8_544 . ?
O1 Co1 O2 81.59(5) . 6 ?
O1 Co1 O2 82.43(5) 8_544 6 ?
O3 Co1 O2 173.49(5) . 6 ?
O1 Co1 O2 92.60(5) . . ?
O1 Co1 O2 80.39(5) 8_544 . ?
O3 Co1 O2 92.49(5) . . ?
O2 Co1 O2 81.035(15) 6 . ?
O1 Co1 C1C 93.68(7) . . ?
O1 Co1 C1C 93.28(7) 8_544 . ?
O3 Co1 C1C 87.52(8) . . ?
O2 Co1 C1C 98.84(8) 6 . ?
O2 Co1 C1C 173.64(7) . . ?
C1 O1 Co1 123.84(10) . . ?
C1 O1 Co1 124.21(9) . 6 ?
Co1 O1 Co1 98.66(5) . 6 ?
C4 O2 Co1 127.40(10) 18_545 8_544 ?
C4 O2 Co1 133.49(10) 18_545 . ?
Co1 O2 Co1 93.03(5) 8_544 . ?
C4 O3 Co1 125.15(10) 13 . ?
O1 C1 C2 118.05(13) . . ?
O1 C1 C3 124.37(13) . 13_556 ?
C2 C1 C3 117.58(13) . 13_556 ?
C3 C2 C1 122.96(14) . . ?
C2 C3 C1 119.46(13) . 13_556 ?
C2 C3 C4 117.01(12) . . ?
C1 C3 C4 123.46(13) 13_556 . ?
O3 C4 O2 123.14(14) 13 17 ?
O3 C4 C3 118.79(13) 13 . ?
O2 C4 C3 118.06(13) 17 . ?
O1C C1C Co1 173.0(3) . . ?
 
_refine_diff_density_max    3.020
_refine_diff_density_min   -1.644
_refine_diff_density_rms    0.236



