#------------------------------------------------------------------------------
#$Date: 2019-10-28 05:32:11 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219729 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/45/4514544.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4514544
loop_
_publ_author_name
'Kim, Hyunuk'
'Sohail, Muhammad'
'Yim, Kanghoon'
'Park, Young Cheol'
'Chun, Dong Hyuk'
'Kim, Hak Joo'
'Han, Seong Ok'
'Moon, Jong-Ho'
_publ_section_title
;
 Effective CO₂ and CO Separation Using [M₂(DOBDC)]
 (M = Mg, Co, Ni) with Unsaturated Metal Sites and Excavation of Their
 Adsorption Sites.
;
_journal_issue                   7
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              7014
_journal_page_last               7021
_journal_paper_doi               10.1021/acsami.8b20450
_journal_volume                  11
_journal_year                    2019
_chemical_formula_sum            'C6 H9 Co O5'
_chemical_formula_weight         220.06
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   26.133(4)
_cell_length_b                   26.133(4)
_cell_length_c                   6.6390(13)
_cell_measurement_reflns_used    176345
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      0.63
_cell_volume                     3926.6(11)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND 4 (Putz & Brandenburg, 2014)'
_computing_publication_material  'enCifer 1.5.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2863
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.978
_diffrn_reflns_theta_min         3.071
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.857
_exptl_absorpt_correction_T_max  2.113
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'HKL3000sm Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       'hexagonal column'
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0499P)²+3.2341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2781
_reflns_number_total             2863
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am8b20450_si_009.cif
_cod_data_source_block           r-3
_cod_original_cell_volume        3926.6(14)
_cod_database_code               4514544
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.524
_shelx_estimated_absorpt_t_max   0.964
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'
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
Co1 Co 0.71951(2) 0.01678(2) 0.32237(2) 0.00190(6) Uani 1 1 d . .
O1 O 0.69274(4) -0.05903(3) 0.16168(11) 0.00309(14) Uani 1 1 d . .
O2 O 0.66007(4) -0.03683(4) 0.53288(12) 0.00411(15) Uani 1 1 d . .
O3 O 0.62970(4) -0.10666(4) 0.76745(12) 0.00518(15) Uani 1 1 d . .
C1 C 0.67984(5) -0.11066(5) 0.25170(16) 0.00331(17) Uani 1 1 d . .
C2 C 0.66021(5) -0.12579(4) 0.45369(16) 0.00320(17) Uani 1 1 d . .
C3 C 0.64962(5) -0.08740(5) 0.59347(16) 0.00320(18) Uani 1 1 d . .
C4 C 0.68556(5) -0.15243(5) 0.13771(16) 0.00403(18) Uani 1 1 d . .
H4A H 0.698556 -0.142984 0.002147 0.005 Uiso 1 1 calc R U
O1M O 0.79017(4) 0.01299(4) 0.46884(14) 0.00968(17) Uani 1 1 d . .
C1M C 0.85198(6) 0.05582(7) 0.4532(2) 0.0153(2) Uani 1 1 d . .
H1M1 H 0.874836 0.035451 0.446058 0.023 Uiso 1 1 calc R U
H1M2 H 0.864321 0.081670 0.571611 0.023 Uiso 1 1 calc R U
H1M3 H 0.858939 0.079562 0.331271 0.023 Uiso 1 1 calc R U
O2M O 0.77548(4) -0.03637(5) 0.84297(15) 0.01264(18) Uani 1 1 d . .
C2M C 0.82650(7) -0.02386(9) 0.9537(3) 0.0248(3) Uani 1 1 d . .
H2M1 H 0.844014 0.015964 1.010866 0.037 Uiso 1 1 calc R U
H2M2 H 0.855163 -0.026136 0.864429 0.037 Uiso 1 1 calc R U
H2M3 H 0.815774 -0.052728 1.062768 0.037 Uiso 1 1 calc R U
H1 H 0.7850(11) -0.0019(11) 0.589(4) 0.026(6) Uiso 1 1 d . .
H5 H 0.7509(11) -0.0426(11) 0.933(4) 0.028(6) Uiso 1 1 d . .
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'
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
O3 Co1 O2 175.58(3) 5_544 .
O3 Co1 O1 93.84(3) 5_544 .
O2 Co1 O1 85.27(3) . .
O3 Co1 O1 94.91(3) 5_544 5_545
O2 Co1 O1 85.23(3) . 5_545
O1 Co1 O1 166.61(3) . 5_545
O3 Co1 O1M 92.36(4) 5_544 .
O2 Co1 O1M 92.03(3) . .
O1 Co1 O1M 94.46(4) . .
O1 Co1 O1M 95.28(3) 5_545 .
O3 Co1 O2 96.85(3) 5_544 9_654
O2 Co1 O2 78.740(12) . 9_654
O1 Co1 O2 81.41(3) . 9_654
O1 Co1 O2 87.50(3) 5_545 9_654
O1M Co1 O2 170.13(3) . 9_654
C1 O1 Co1 121.99(7) . .
C1 O1 Co1 120.68(7) . 9_654
Co1 O1 Co1 96.65(3) . 9_654
C3 O2 Co1 128.64(7) . .
C3 O2 Co1 136.31(7) . 5_545
Co1 O2 Co1 92.26(3) . 5_545
C3 O3 Co1 121.85(7) . 9_655
O1 C1 C4 117.95(9) . .
O1 C1 C2 124.70(9) . .
C4 C1 C2 117.34(9) . .
C4 C2 C1 119.28(9) 16_645 .
C4 C2 C3 116.38(9) 16_645 .
C1 C2 C3 124.31(9) . .
O3 C3 O2 122.27(10) . .
O3 C3 C2 118.64(9) . .
O2 C3 C2 119.08(9) . .
C1 C4 C2 123.38(9) . 16_645
C1M O1M Co1 126.37(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.0271(9) 5_544
Co1 O2 2.0378(8) .
Co1 O1 2.0413(8) .
Co1 O1 2.0590(8) 5_545
Co1 O1M 2.1327(9) .
Co1 O2 2.2073(9) 9_654
O1 C1 1.3551(13) .
O2 C3 1.2736(13) .
O3 C3 1.2635(13) .
C1 C4 1.3965(14) .
C1 C2 1.4195(14) .
C2 C4 1.4006(14) 16_645
C2 C3 1.4904(14) .
O1M C1M 1.4369(16) .
O2M C2M 1.4104(18) .
