#------------------------------------------------------------------------------
#$Date: 2019-10-28 05:33:01 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219732 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/45/4514547.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_4514547
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            'C5.56 H Co O4.56'
_chemical_formula_weight         199.67
_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   geom
_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                   25.844(4)
_cell_length_b                   25.844(4)
_cell_length_c                   6.8710(14)
_cell_measurement_reflns_used    127237
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      0.57
_cell_volume                     3974.4(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.887
_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     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4344
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         37.625
_diffrn_reflns_theta_min         3.054
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  1.294
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'HKL3000sm Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       'hexagonal column'
_exptl_crystal_F_000             1761
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.020
_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.236
_refine_ls_extinction_coef       0.045(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         4344
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1416P)²+0.3723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3968
_reflns_number_total             4344
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am8b20450_si_006.cif
_cod_data_source_block           r-3
_cod_original_cell_volume        3974.5(14)
_cod_database_code               4514547
_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   0.825
_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
_atom_site_refinement_flags_occupancy
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
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
