 
data_R-3m
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Co O2 Pd' 
_chemical_formula_weight          197.33

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0106   0.0060
 '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'
 'Pd'  'Pd'  -0.9988   1.0072
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            166
_space_group_name_H-M_alt         'R -3 m :H'
_space_group_name_Hall            '-R 3 2"'
 
_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'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -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'
 'y+2/3, x+1/3, -z+1/3'
 'x-y+2/3, -y+1/3, -z+1/3'
 '-x+2/3, -x+y+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'
 'y+1/3, x+2/3, -z+2/3'
 'x-y+1/3, -y+2/3, -z+2/3'
 '-x+1/3, -x+y+2/3, -z+2/3'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, 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'
 '-y+2/3, -x+1/3, z+1/3'
 '-x+y+2/3, y+1/3, z+1/3'
 'x+2/3, x-y+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'
 '-y+1/3, -x+2/3, z+2/3'
 '-x+y+1/3, y+2/3, z+2/3'
 'x+1/3, x-y+2/3, z+2/3'
 
_cell_length_a                    2.845(3)
_cell_length_b                    2.845(3)
_cell_length_c                    17.880(16)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      125.3(3)
_cell_formula_units_Z             1
_cell_measurement_temperature     295(2)
_cell_measurement_reflns_used     360
_cell_measurement_theta_min       6.837
_cell_measurement_theta_max       80.556
 
_exptl_crystal_description        'prism'
_exptl_crystal_colour             'black'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.615          
_exptl_crystal_F_000              89
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.100
_exptl_crystal_size_mid           0.080
_exptl_crystal_size_min           0.050
_exptl_absorpt_coefficient_mu     6.731
_shelx_estimated_absorpt_T_min    0.553
_shelx_estimated_absorpt_T_max    0.730
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.1637
_exptl_absorpt_correction_T_max   0.2795
_exptl_absorpt_process_details    'SAD2ABS-2014/4 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       295(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker D8 Venture; Photon100 area detector'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             389
_diffrn_reflns_av_unetI/netI      0.0286
_diffrn_reflns_av_R_equivalents   0.0300
_diffrn_reflns_limit_h_min        -4
_diffrn_reflns_limit_h_max        5
_diffrn_reflns_limit_k_min        -3
_diffrn_reflns_limit_k_max        4
_diffrn_reflns_limit_l_min        -31
_diffrn_reflns_limit_l_max        31
_diffrn_reflns_theta_min          3.418
_diffrn_reflns_theta_max          40.276
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.879
_diffrn_measured_fraction_theta_full  0.977
_diffrn_reflns_Laue_measured_fraction_max    0.879
_diffrn_reflns_Laue_measured_fraction_full   0.977
_diffrn_reflns_point_group_measured_fraction_max   0.879
_diffrn_reflns_point_group_measured_fraction_full  0.977
_reflns_number_total              116
_reflns_number_gt                 116
_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-2016/6 (Sheldrick, 2016)'
_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)+(0.0456P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef        0.027(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          116
_refine_ls_number_parameters      9
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0297
_refine_ls_R_factor_gt            0.0297
_refine_ls_wR_factor_ref          0.0709
_refine_ls_wR_factor_gt           0.0709
_refine_ls_goodness_of_fit_ref    1.299
_refine_ls_restrained_S_all       1.299
_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
Pd1 Pd 0.000000 0.000000 0.000000 0.0052(2) Uani 1 12 d S T P . .
Co2 Co 0.333333 -0.333333 0.166667 0.0042(3) Uani 1 12 d S T P . .
O3 O 0.000000 0.000000 0.11215(16) 0.0054(6) Uani 1 6 d S T 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
Pd1 O3 2.005(3) . ?
Pd1 O3 2.005(3) 19 ?
Pd1 Pd1 2.845(3) 1_445 ?
Pd1 Pd1 2.845(3) 1_665 ?
Pd1 Pd1 2.845(3) 1_545 ?
Pd1 Pd1 2.845(3) 1_655 ?
Pd1 Pd1 2.845(3) 1_565 ?
Pd1 Pd1 2.845(3) 1_455 ?
Co2 O3 1.910(2) 1_545 ?
Co2 O3 1.910(2) 1_655 ?
Co2 O3 1.910(2) . ?
Co2 O3 1.910(2) 25_545 ?
Co2 O3 1.910(2) 25 ?
Co2 O3 1.910(2) 25_445 ?
Co2 Co2 2.845(3) 25_645 ?
Co2 Co2 2.845(3) 1_565 ?
Co2 Co2 2.845(3) 1_455 ?
Co2 Co2 2.845(3) 1_445 ?
Co2 Co2 2.845(3) 25_655 ?
Co2 Co2 2.845(3) 1_545 ?
 
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 Pd1 O3 180.0 . 19 ?
O3 Pd1 Pd1 90.0 . 1_445 ?
O3 Pd1 Pd1 90.0 19 1_445 ?
O3 Pd1 Pd1 90.0 . 1_665 ?
O3 Pd1 Pd1 90.0 19 1_665 ?
Pd1 Pd1 Pd1 180.0 1_445 1_665 ?
O3 Pd1 Pd1 90.0 . 1_545 ?
O3 Pd1 Pd1 90.0 19 1_545 ?
Pd1 Pd1 Pd1 60.0 1_445 1_545 ?
Pd1 Pd1 Pd1 120.0 1_665 1_545 ?
O3 Pd1 Pd1 90.0 . 1_655 ?
O3 Pd1 Pd1 90.0 19 1_655 ?
Pd1 Pd1 Pd1 120.0 1_445 1_655 ?
Pd1 Pd1 Pd1 60.0 1_665 1_655 ?
Pd1 Pd1 Pd1 60.0 1_545 1_655 ?
O3 Pd1 Pd1 90.0 . 1_565 ?
O3 Pd1 Pd1 90.0 19 1_565 ?
Pd1 Pd1 Pd1 120.0 1_445 1_565 ?
Pd1 Pd1 Pd1 60.0 1_665 1_565 ?
Pd1 Pd1 Pd1 180.0 1_545 1_565 ?
Pd1 Pd1 Pd1 120.0 1_655 1_565 ?
O3 Pd1 Pd1 90.0 . 1_455 ?
O3 Pd1 Pd1 90.0 19 1_455 ?
Pd1 Pd1 Pd1 60.0 1_445 1_455 ?
Pd1 Pd1 Pd1 120.0 1_665 1_455 ?
Pd1 Pd1 Pd1 120.0 1_545 1_455 ?
Pd1 Pd1 Pd1 180.0 1_655 1_455 ?
Pd1 Pd1 Pd1 60.0 1_565 1_455 ?
O3 Co2 O3 96.28(11) 1_545 1_655 ?
O3 Co2 O3 96.28(10) 1_545 . ?
O3 Co2 O3 96.28(11) 1_655 . ?
O3 Co2 O3 83.72(11) 1_545 25_545 ?
O3 Co2 O3 83.72(11) 1_655 25_545 ?
O3 Co2 O3 180.0 . 25_545 ?
O3 Co2 O3 180.0 1_545 25 ?
O3 Co2 O3 83.72(11) 1_655 25 ?
O3 Co2 O3 83.72(11) . 25 ?
O3 Co2 O3 96.27(11) 25_545 25 ?
O3 Co2 O3 83.72(11) 1_545 25_445 ?
O3 Co2 O3 180.0 1_655 25_445 ?
O3 Co2 O3 83.72(11) . 25_445 ?
O3 Co2 O3 96.27(11) 25_545 25_445 ?
O3 Co2 O3 96.27(11) 25 25_445 ?
O3 Co2 Co2 90.0 1_545 25_645 ?
O3 Co2 Co2 41.86(5) 1_655 25_645 ?
O3 Co2 Co2 138.14(5) . 25_645 ?
O3 Co2 Co2 41.86(5) 25_545 25_645 ?
O3 Co2 Co2 90.0 25 25_645 ?
O3 Co2 Co2 138.14(5) 25_445 25_645 ?
O3 Co2 Co2 138.14(5) 1_545 1_565 ?
O3 Co2 Co2 90.0 1_655 1_565 ?
O3 Co2 Co2 41.86(5) . 1_565 ?
O3 Co2 Co2 138.14(5) 25_545 1_565 ?
O3 Co2 Co2 41.86(5) 25 1_565 ?
O3 Co2 Co2 90.0 25_445 1_565 ?
Co2 Co2 Co2 120.0 25_645 1_565 ?
O3 Co2 Co2 90.0 1_545 1_455 ?
O3 Co2 Co2 138.14(5) 1_655 1_455 ?
O3 Co2 Co2 41.86(5) . 1_455 ?
O3 Co2 Co2 138.14(5) 25_545 1_455 ?
O3 Co2 Co2 90.0 25 1_455 ?
O3 Co2 Co2 41.86(5) 25_445 1_455 ?
Co2 Co2 Co2 180.0 25_645 1_455 ?
Co2 Co2 Co2 60.0 1_565 1_455 ?
O3 Co2 Co2 41.86(5) 1_545 1_445 ?
O3 Co2 Co2 138.14(5) 1_655 1_445 ?
O3 Co2 Co2 90.0 . 1_445 ?
O3 Co2 Co2 90.0 25_545 1_445 ?
O3 Co2 Co2 138.14(5) 25 1_445 ?
O3 Co2 Co2 41.86(5) 25_445 1_445 ?
Co2 Co2 Co2 120.0 25_645 1_445 ?
Co2 Co2 Co2 120.0 1_565 1_445 ?
Co2 Co2 Co2 60.0 1_455 1_445 ?
O3 Co2 Co2 138.14(5) 1_545 25_655 ?
O3 Co2 Co2 41.86(5) 1_655 25_655 ?
O3 Co2 Co2 90.0 . 25_655 ?
O3 Co2 Co2 90.0 25_545 25_655 ?
O3 Co2 Co2 41.86(5) 25 25_655 ?
O3 Co2 Co2 138.14(5) 25_445 25_655 ?
Co2 Co2 Co2 60.0 25_645 25_655 ?
Co2 Co2 Co2 60.0 1_565 25_655 ?
Co2 Co2 Co2 120.0 1_455 25_655 ?
Co2 Co2 Co2 180.0 1_445 25_655 ?
O3 Co2 Co2 41.86(5) 1_545 1_545 ?
O3 Co2 Co2 90.0 1_655 1_545 ?
O3 Co2 Co2 138.14(5) . 1_545 ?
O3 Co2 Co2 41.86(5) 25_545 1_545 ?
O3 Co2 Co2 138.14(5) 25 1_545 ?
O3 Co2 Co2 90.0 25_445 1_545 ?
Co2 Co2 Co2 60.0 25_645 1_545 ?
Co2 Co2 Co2 180.0 1_565 1_545 ?
Co2 Co2 Co2 120.0 1_455 1_545 ?
Co2 Co2 Co2 60.000(1) 1_445 1_545 ?
Co2 Co2 Co2 120.0 25_655 1_545 ?
Co2 O3 Co2 96.28(11) 1_565 1_455 ?
Co2 O3 Co2 96.28(11) 1_565 . ?
Co2 O3 Co2 96.28(11) 1_455 . ?
Co2 O3 Pd1 120.69(8) 1_565 . ?
Co2 O3 Pd1 120.69(8) 1_455 . ?
Co2 O3 Pd1 120.69(8) . . ?
 
_refine_diff_density_max    1.806
_refine_diff_density_min   -1.937
_refine_diff_density_rms    0.635



