#------------------------------------------------------------------------------
#$Date: 2019-10-28 05:33:58 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219735 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/45/4514550.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_4514550
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            'C14 H20.33 Ni2 O12.17'
_chemical_formula_weight         500.72
_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                   25.871(4)
_cell_length_b                   25.871(4)
_cell_length_c                   13.500(3)
_cell_measurement_reflns_used    176910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      0.63
_cell_volume                     7825(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5309
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_min         1.735
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    2.136
_exptl_absorpt_correction_T_max  75.683
_exptl_absorpt_correction_T_min  0.0128
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'HKL3000sm Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_description       'hexagonal column'
_exptl_crystal_F_000             4638
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         5.246
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         5309
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2932
_refine_ls_wR_factor_ref         0.3197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4200
_reflns_number_total             5309
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am8b20450_si_012.cif
_cod_data_source_block           r-3
_cod_original_cell_volume        7825(3)
_cod_database_code               4514550
_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   0.848
_shelx_estimated_absorpt_t_max   0.919
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
Ni1 Ni 0.61872(2) 0.96686(2) 1.07701(4) 0.0143(2) Uani 1 1 d . . .
Ni2 Ni 0.68481(2) 1.05157(2) 1.24040(4) 0.0143(2) Uani 1 1 d . . .
O1 O 0.67683(15) 0.97322(14) 1.1820(2) 0.0162(6) Uani 1 1 d . . .
O2 O 0.64265(15) 0.91583(15) 1.0008(2) 0.0158(6) Uani 1 1 d . . .
O3 O 0.69855(15) 0.92924(15) 1.3037(2) 0.0170(6) Uani 1 1 d . . .
O4 O 0.69436(15) 0.75136(15) 1.1722(2) 0.0162(6) Uani 1 1 d . . .
O5 O 0.63835(16) 0.74045(14) 0.8692(2) 0.0175(6) Uani 1 1 d . . .
O6 O 0.66130(15) 0.69630(14) 0.9880(2) 0.0159(6) Uani 1 1 d . . .
C1 C 0.68348(19) 0.93060(18) 1.2152(3) 0.0150(7) Uani 1 1 d . . .
C2 C 0.6565(2) 0.87782(19) 1.0459(3) 0.0174(7) Uani 1 1 d . . .
C3 C 0.6740(2) 0.88138(19) 1.1468(3) 0.0163(7) Uani 1 1 d . . .
C4 C 0.6853(2) 0.83701(19) 1.1844(3) 0.0178(8) Uani 1 1 d . . .
H4 H 0.696339 0.839318 1.252084 0.021 Uiso 1 1 calc R U .
C5 C 0.6813(2) 0.79004(19) 1.1278(3) 0.0158(7) Uani 1 1 d . . .
C6 C 0.6638(2) 0.7873(2) 1.0270(3) 0.0172(8) Uani 1 1 d . . .
C7 C 0.6526(2) 0.83133(19) 0.9892(3) 0.0178(8) Uani 1 1 d . . .
H7 H 0.641937 0.829185 0.921387 0.021 Uiso 1 1 calc R U .
C8 C 0.65396(19) 0.73828(19) 0.9565(3) 0.0155(7) Uani 1 1 d . . .
O1E O 0.54876(18) 0.89504(18) 1.1475(3) 0.0296(8) Uani 1 1 d . U .
H1E H 0.553376 0.929425 1.141705 0.044 Uiso 1 1 calc R U .
O2E O 0.5291(4) 0.8331(5) 0.9508(8) 0.129(3) Uani 1 1 d . U .
H2E H 0.565666 0.854455 0.963272 0.194 Uiso 1 1 calc R U .
C1E C 0.4944(5) 0.8541(5) 1.1102(7) 0.119(4) Uani 1 1 d D U .
H1E1 H 0.477846 0.875452 1.072802 0.143 Uiso 1 1 calc R U .
H1E2 H 0.467049 0.833240 1.166143 0.143 Uiso 1 1 calc R U .
C2E C 0.4958(8) 0.8090(6) 1.0444(10) 0.169(7) Uani 1 1 d D U .
H2E1 H 0.454215 0.778443 1.028111 0.202 Uiso 1 1 calc R U .
H2E2 H 0.513922 0.788918 1.081031 0.202 Uiso 1 1 calc R U .
O3E O 0.6873(2) 1.12786(19) 1.2952(3) 0.0330(9) Uani 1 1 d . U .
H3E H 0.688291 1.149851 1.248510 0.050 Uiso 1 1 calc R U .
O4E O 0.6873(6) 1.2389(5) 1.3472(9) 0.153(4) Uani 1 1 d . U .
H4E H 0.651303 1.229020 1.339543 0.229 Uiso 1 1 calc R U .
C3E C 0.6629(4) 1.1388(4) 1.3783(6) 0.0657(19) Uani 1 1 d . U .
H3E1 H 0.663901 1.113915 1.433177 0.079 Uiso 1 1 calc R U .
H3E2 H 0.620400 1.125195 1.364329 0.079 Uiso 1 1 calc R U .
C4E C 0.6913(7) 1.2004(5) 1.4123(9) 0.107(4) Uani 1 1 d . U .
H4E1 H 0.672786 1.201571 1.475857 0.129 Uiso 1 1 calc R U .
H4E2 H 0.733978 1.214532 1.425329 0.129 Uiso 1 1 calc R U .
O5E O 0.3614(2) 0.8853(2) 0.9944(4) 0.0509(12) Uani 1 1 d . U .
H5E H 0.353910 0.875045 1.054024 0.076 Uiso 1 1 calc R U .
O6E O 0.2752(7) 0.7890(6) 0.8673(8) 0.186(6) Uani 1 1 d . U .
H6E H 0.268786 0.817096 0.880354 0.279 Uiso 1 1 calc R U .
C5E C 0.3560(8) 0.8389(6) 0.9400(12) 0.144(5) Uani 1 1 d D U .
H5E1 H 0.390948 0.834468 0.955440 0.172 Uiso 1 1 calc R U .
H5E2 H 0.359537 0.850789 0.869556 0.172 Uiso 1 1 calc R U .
C6E C 0.3022(9) 0.7787(7) 0.9487(16) 0.206(8) Uani 1 1 d D U .
H6E1 H 0.280007 0.772811 1.011323 0.247 Uiso 1 1 calc R U .
H6E2 H 0.310638 0.745835 0.937896 0.247 Uiso 1 1 calc R U .
O1W O 0.333333 0.666667 1.166667 0.588(13) Uani 1 6 d S TU 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'
Ni Ni 0.2288 1.0875 '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
O2 Ni1 O1 87.19(12) . .
O2 Ni1 O3 95.39(13) . 9_564
O1 Ni1 O3 175.15(14) . 9_564
O2 Ni1 O4 170.01(13) . 15_557
O1 Ni1 O4 85.10(13) . 15_557
O3 Ni1 O4 91.87(13) 9_564 15_557
O2 Ni1 O6 81.78(13) . 11_567
O1 Ni1 O6 82.15(9) . 11_567
O3 Ni1 O6 94.13(13) 9_564 11_567
O4 Ni1 O6 90.87(13) 15_557 11_567
O2 Ni1 Ni2 127.88(10) . .
O1 Ni1 Ni2 44.49(9) . .
O3 Ni1 Ni2 131.51(10) 9_564 .
O4 Ni1 Ni2 42.83(9) 15_557 .
O6 Ni1 Ni2 74.57(9) 11_567 .
O6 Ni2 O4 87.05(13) 15_557 15_557
O6 Ni2 O5 173.90(14) 15_557 11_567
O4 Ni2 O5 94.28(13) 15_557 11_567
O6 Ni2 O2 82.63(13) 15_557 5_665
O4 Ni2 O2 168.86(13) 15_557 5_665
O5 Ni2 O2 95.55(13) 11_567 5_665
O6 Ni2 O1 81.70(9) 15_557 .
O4 Ni2 O1 83.71(14) 15_557 .
O5 Ni2 O1 92.52(13) 11_567 .
O2 Ni2 O1 90.63(12) 5_665 .
O6 Ni2 Ni1 93.00(10) 15_557 .
O4 Ni2 Ni1 43.37(9) 15_557 .
O5 Ni2 Ni1 83.95(9) 11_567 .
O2 Ni2 Ni1 132.82(9) 5_665 .
O1 Ni2 Ni1 42.50(9) . .
C1 O1 Ni1 126.4(3) . .
C1 O1 Ni2 135.6(3) . .
Ni1 O1 Ni2 93.01(13) . .
C2 O2 Ni1 122.1(3) . .
C2 O2 Ni2 122.8(3) . 9_564
Ni1 O2 Ni2 95.88(14) . 9_564
C1 O3 Ni1 123.1(3) . 5_665
C5 O4 Ni2 121.6(2) . 14_457
C5 O4 Ni1 122.4(3) . 14_457
Ni2 O4 Ni1 93.80(14) 14_457 14_457
C8 O5 Ni2 124.3(3) . 12_657
C8 O6 Ni2 127.9(3) . 14_457
C8 O6 Ni1 133.5(3) . 12_657
Ni2 O6 Ni1 94.23(14) 14_457 12_657
O3 C1 O1 122.1(4) . .
O3 C1 C3 118.9(4) . .
O1 C1 C3 119.0(3) . .
O2 C2 C7 116.9(4) . .
O2 C2 C3 125.2(4) . .
C7 C2 C3 117.8(4) . .
C4 C3 C2 118.7(4) . .
C4 C3 C1 117.4(4) . .
C2 C3 C1 123.9(4) . .
C5 C4 C3 123.7(4) . .
O4 C5 C4 117.8(4) . .
O4 C5 C6 125.4(4) . .
C4 C5 C6 116.8(4) . .
C7 C6 C5 119.7(4) . .
C7 C6 C8 116.0(4) . .
C5 C6 C8 124.3(4) . .
C2 C7 C6 123.2(4) . .
O5 C8 O6 122.9(4) . .
O5 C8 C6 118.6(4) . .
O6 C8 C6 118.5(3) . .
O1E C1E C2E 114.3(11) . .
C1E C2E O2E 114.8(11) . .
O3E C3E C4E 116.5(9) . .
O4E C4E C3E 114.3(11) . .
O5E C5E C6E 121.0(15) . .
C5E C6E O6E 92.0(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.001(3) .
Ni1 O1 2.012(3) .
Ni1 O3 2.030(3) 9_564
Ni1 O4 2.047(3) 15_557
Ni1 O6 2.090(3) 11_567
Ni1 Ni2 2.9739(8) .
Ni2 O6 2.011(3) 15_557
Ni2 O4 2.026(3) 15_557
Ni2 O5 2.022(3) 11_567
Ni2 O2 2.046(3) 5_665
Ni2 O1 2.087(3) .
O1 C1 1.279(5) .
O2 C2 1.349(5) .
O3 C1 1.263(5) .
O4 C5 1.347(5) .
O5 C8 1.256(5) .
O6 C8 1.266(5) .
C1 C3 1.491(6) .
C2 C7 1.387(6) .
C2 C3 1.424(6) .
C3 C4 1.413(6) .
C4 C5 1.394(6) .
C5 C6 1.425(5) .
C6 C7 1.404(6) .
C6 C8 1.502(6) .
O1E C1E 1.365(10) .
O2E C2E 1.480(17) .
C1E C2E 1.481(9) .
O3E C3E 1.384(8) .
O4E C4E 1.371(15) .
C3E C4E 1.456(13) .
O5E C5E 1.353(13) .
O6E C6E 1.40(2) .
C5E C6E 1.486(10) .
