data_publication_text
_publ_requested_journal          J.Am.Chem.Soc.
_publ_contact_author_name        'Nak Cheon Jeong'
_publ_contact_author_address     
'Department of Emerging Materials Science, DGIST, Daegu 711-873, Korea'
_publ_contact_author_email       nc@dgist.ac.kr
_publ_contact_author_phone       82-53-785-6513
_publ_contact_author_fax         82-53-785-6509
loop_
_publ_author_name
_publ_author_address
'Jeong, Nak Cheon '
'Department of Emerging Materials Science, DGIST, Daegu 711-873, Korea'
'Song, Dahae'
'Department of Emerging Materials Science, DGIST, Daegu 711-873, Korea'
'Bae, Jinhee'
'Department of Emerging Materials Science, DGIST, Daegu 711-873, Korea'
'Ji, Hoon'
'Department of Emerging Materials Science, DGIST, Daegu 711-873, Korea'
'Kim, Min-Bum'
'Department of Chemical and Biomolecular Engineering, Yonsei University, Seoul 120-749, Korea '
'Bae, Youn-Sang'
'Department of Chemical and Biomolecular Engineering, Yonsei University, Seoul 120-749, Korea '
'Moon, Dohyun'
'Beamline Department, Pohang Accelerator Laboratory, Pohang 37673, Korea'
 
data_Pristine-HK
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C144 H96 Cu24 O120, +[Solvent]'
_chemical_formula_sum
 'C144 H96 Cu24 O120' 
_chemical_formula_weight          5271.16

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0019   0.0011
 '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'   0.0074   0.0043
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cu'  'Cu'   0.3373   0.9674
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       cubic
_space_group_IT_number            225
_space_group_name_H-M_alt         'F m -3 m'
_space_group_name_Hall            '-F 4 2 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'
 '-x, -y, z'
 '-x, y, -z'
 'x, -y, -z'
 'z, x, y'
 'z, -x, -y'
 '-z, -x, y'
 '-z, x, -y'
 'y, z, x'
 '-y, z, -x'
 'y, -z, -x'
 '-y, -z, x'
 'y, x, -z'
 '-y, -x, -z'
 'y, -x, z'
 '-y, x, z'
 'x, z, -y'
 '-x, z, y'
 '-x, -z, -y'
 'x, -z, y'
 'z, y, -x'
 'z, -y, x'
 '-z, y, x'
 '-z, -y, -x'
 'x, y+1/2, z+1/2'
 '-x, -y+1/2, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x, -y+1/2, -z+1/2'
 'z, x+1/2, y+1/2'
 'z, -x+1/2, -y+1/2'
 '-z, -x+1/2, y+1/2'
 '-z, x+1/2, -y+1/2'
 'y, z+1/2, x+1/2'
 '-y, z+1/2, -x+1/2'
 'y, -z+1/2, -x+1/2'
 '-y, -z+1/2, x+1/2'
 'y, x+1/2, -z+1/2'
 '-y, -x+1/2, -z+1/2'
 'y, -x+1/2, z+1/2'
 '-y, x+1/2, z+1/2'
 'x, z+1/2, -y+1/2'
 '-x, z+1/2, y+1/2'
 '-x, -z+1/2, -y+1/2'
 'x, -z+1/2, y+1/2'
 'z, y+1/2, -x+1/2'
 'z, -y+1/2, x+1/2'
 '-z, y+1/2, x+1/2'
 '-z, -y+1/2, -x+1/2'
 'x+1/2, y, z+1/2'
 '-x+1/2, -y, z+1/2'
 '-x+1/2, y, -z+1/2'
 'x+1/2, -y, -z+1/2'
 'z+1/2, x, y+1/2'
 'z+1/2, -x, -y+1/2'
 '-z+1/2, -x, y+1/2'
 '-z+1/2, x, -y+1/2'
 'y+1/2, z, x+1/2'
 '-y+1/2, z, -x+1/2'
 'y+1/2, -z, -x+1/2'
 '-y+1/2, -z, x+1/2'
 'y+1/2, x, -z+1/2'
 '-y+1/2, -x, -z+1/2'
 'y+1/2, -x, z+1/2'
 '-y+1/2, x, z+1/2'
 'x+1/2, z, -y+1/2'
 '-x+1/2, z, y+1/2'
 '-x+1/2, -z, -y+1/2'
 'x+1/2, -z, y+1/2'
 'z+1/2, y, -x+1/2'
 'z+1/2, -y, x+1/2'
 '-z+1/2, y, x+1/2'
 '-z+1/2, -y, -x+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, -z'
 'z+1/2, x+1/2, y'
 'z+1/2, -x+1/2, -y'
 '-z+1/2, -x+1/2, y'
 '-z+1/2, x+1/2, -y'
 'y+1/2, z+1/2, x'
 '-y+1/2, z+1/2, -x'
 'y+1/2, -z+1/2, -x'
 '-y+1/2, -z+1/2, x'
 'y+1/2, x+1/2, -z'
 '-y+1/2, -x+1/2, -z'
 'y+1/2, -x+1/2, z'
 '-y+1/2, x+1/2, z'
 'x+1/2, z+1/2, -y'
 '-x+1/2, z+1/2, y'
 '-x+1/2, -z+1/2, -y'
 'x+1/2, -z+1/2, y'
 'z+1/2, y+1/2, -x'
 'z+1/2, -y+1/2, x'
 '-z+1/2, y+1/2, x'
 '-z+1/2, -y+1/2, -x'
 '-x, -y, -z'
 'x, y, -z'
 'x, -y, z'
 '-x, y, z'
 '-z, -x, -y'
 '-z, x, y'
 'z, x, -y'
 'z, -x, y'
 '-y, -z, -x'
 'y, -z, x'
 '-y, z, x'
 'y, z, -x'
 '-y, -x, z'
 'y, x, z'
 '-y, x, -z'
 'y, -x, -z'
 '-x, -z, y'
 'x, -z, -y'
 'x, z, y'
 '-x, z, -y'
 '-z, -y, x'
 '-z, y, -x'
 'z, -y, -x'
 'z, y, x'
 '-x, -y+1/2, -z+1/2'
 'x, y+1/2, -z+1/2'
 'x, -y+1/2, z+1/2'
 '-x, y+1/2, z+1/2'
 '-z, -x+1/2, -y+1/2'
 '-z, x+1/2, y+1/2'
 'z, x+1/2, -y+1/2'
 'z, -x+1/2, y+1/2'
 '-y, -z+1/2, -x+1/2'
 'y, -z+1/2, x+1/2'
 '-y, z+1/2, x+1/2'
 'y, z+1/2, -x+1/2'
 '-y, -x+1/2, z+1/2'
 'y, x+1/2, z+1/2'
 '-y, x+1/2, -z+1/2'
 'y, -x+1/2, -z+1/2'
 '-x, -z+1/2, y+1/2'
 'x, -z+1/2, -y+1/2'
 'x, z+1/2, y+1/2'
 '-x, z+1/2, -y+1/2'
 '-z, -y+1/2, x+1/2'
 '-z, y+1/2, -x+1/2'
 'z, -y+1/2, -x+1/2'
 'z, y+1/2, x+1/2'
 '-x+1/2, -y, -z+1/2'
 'x+1/2, y, -z+1/2'
 'x+1/2, -y, z+1/2'
 '-x+1/2, y, z+1/2'
 '-z+1/2, -x, -y+1/2'
 '-z+1/2, x, y+1/2'
 'z+1/2, x, -y+1/2'
 'z+1/2, -x, y+1/2'
 '-y+1/2, -z, -x+1/2'
 'y+1/2, -z, x+1/2'
 '-y+1/2, z, x+1/2'
 'y+1/2, z, -x+1/2'
 '-y+1/2, -x, z+1/2'
 'y+1/2, x, z+1/2'
 '-y+1/2, x, -z+1/2'
 'y+1/2, -x, -z+1/2'
 '-x+1/2, -z, y+1/2'
 'x+1/2, -z, -y+1/2'
 'x+1/2, z, y+1/2'
 '-x+1/2, z, -y+1/2'
 '-z+1/2, -y, x+1/2'
 '-z+1/2, y, -x+1/2'
 'z+1/2, -y, -x+1/2'
 'z+1/2, y, x+1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z'
 '-z+1/2, -x+1/2, -y'
 '-z+1/2, x+1/2, y'
 'z+1/2, x+1/2, -y'
 'z+1/2, -x+1/2, y'
 '-y+1/2, -z+1/2, -x'
 'y+1/2, -z+1/2, x'
 '-y+1/2, z+1/2, x'
 'y+1/2, z+1/2, -x'
 '-y+1/2, -x+1/2, z'
 'y+1/2, x+1/2, z'
 '-y+1/2, x+1/2, -z'
 'y+1/2, -x+1/2, -z'
 '-x+1/2, -z+1/2, y'
 'x+1/2, -z+1/2, -y'
 'x+1/2, z+1/2, y'
 '-x+1/2, z+1/2, -y'
 '-z+1/2, -y+1/2, x'
 '-z+1/2, y+1/2, -x'
 'z+1/2, -y+1/2, -x'
 'z+1/2, y+1/2, x'
 
_cell_length_a                    26.274(3)
_cell_length_b                    26.274(3)
_cell_length_c                    26.274(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      18137(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     108608
_cell_measurement_theta_min       0.350
_cell_measurement_theta_max       33.679
 
_exptl_crystal_description        'octahedron'
_exptl_crystal_colour             'blue'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     0.965          
_exptl_crystal_F_000              5232
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.315
_exptl_crystal_size_mid           0.305
_exptl_crystal_size_min           0.298
_exptl_absorpt_coefficient_mu     0.944
_shelx_estimated_absorpt_T_min    0.755
_shelx_estimated_absorpt_T_max    0.766
_exptl_absorpt_correction_type    'empirical'
_exptl_absorpt_correction_T_min   0.946
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.610
_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             40493
_diffrn_reflns_av_unetI/netI      0.0195
_diffrn_reflns_av_R_equivalents   0.0765
_diffrn_reflns_limit_h_min        -36
_diffrn_reflns_limit_h_max        36
_diffrn_reflns_limit_k_min        -36
_diffrn_reflns_limit_k_max        36
_diffrn_reflns_limit_l_min        -36
_diffrn_reflns_limit_l_max        36
_diffrn_reflns_theta_min          1.152
_diffrn_reflns_theta_max          24.986
_diffrn_reflns_theta_full         21.469
_diffrn_measured_fraction_theta_max   0.995
_diffrn_measured_fraction_theta_full  0.993
_diffrn_reflns_Laue_measured_fraction_max    0.995
_diffrn_reflns_Laue_measured_fraction_full   0.993
_diffrn_reflns_point_group_measured_fraction_max   0.995
_diffrn_reflns_point_group_measured_fraction_full  0.993
_reflns_number_total              1315
_reflns_number_gt                 1142
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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        '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     'SHELXT-2018(Sheldrick, 2018)'
_computing_structure_refinement   'SHELXL-2018(Sheldrick, 2018)'
_computing_molecular_graphics     'DIAMOND 4(Putx&Brandenburg, 2014)'
_computing_publication_material   'publCIF(Westrip, 2010)'
_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)+(0.0629P)²+14.5303P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.00042(6)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          1315
_refine_ls_number_parameters      39
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0399
_refine_ls_R_factor_gt            0.0342
_refine_ls_wR_factor_ref          0.1000
_refine_ls_wR_factor_gt           0.0977
_refine_ls_goodness_of_fit_ref    1.111
_refine_ls_restrained_S_all       1.114
_refine_ls_shift/su_max           0.001
_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
Cu1 Cu 0.500000 0.28527(2) 0.28527(2) 0.02478(16) Uani 1 4 d S T P . .
O1 O 0.44758(5) 0.24345(5) 0.31703(5) 0.0389(3) Uani 1 1 d . . . . .
O2 O 0.500000 0.34358(8) 0.34358(8) 0.1086(17) Uani 1 4 d DS T P . .
H1O2 H 0.500000 0.3430(11) 0.3819(7) 0.163 Uiso 1 2 d DS U P . .
C1 C 0.43116(9) 0.20294(7) 0.29706(7) 0.0327(4) Uani 1 2 d S T P . .
C2 C 0.38712(8) 0.17745(7) 0.32255(7) 0.0326(5) Uani 1 2 d S T P . .
C3 C 0.36576(6) 0.19896(9) 0.36576(6) 0.0334(5) Uani 1 2 d S T P . .
H3 H 0.380678 0.228324 0.380679 0.040 Uiso 1 2 calc R 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
Cu1 O1 1.9495(12) . ?
Cu1 O1 1.9496(12) 115 ?
Cu1 O1 1.9496(12) 18_655 ?
Cu1 O1 1.9496(12) 100_655 ?
Cu1 O2 2.166(3) . ?
Cu1 Cu1 2.6212(7) 121_655 ?
O1 C1 1.2626(16) . ?
O2 H1O2 1.008(18) . ?
O2 H1O2 1.008(18) 18_655 ?
C1 C2 1.495(3) . ?
C2 C3 1.3869(17) . ?
C2 C3 1.3869(17) 30 ?
C3 H3 0.9500 . ?
 
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 Cu1 O1 89.05(8) . 115 ?
O1 Cu1 O1 168.99(7) . 18_655 ?
O1 Cu1 O1 89.89(8) 115 18_655 ?
O1 Cu1 O1 89.90(8) . 100_655 ?
O1 Cu1 O1 168.99(7) 115 100_655 ?
O1 Cu1 O1 89.05(8) 18_655 100_655 ?
O1 Cu1 O2 95.51(4) . . ?
O1 Cu1 O2 95.51(4) 115 . ?
O1 Cu1 O2 95.51(4) 18_655 . ?
O1 Cu1 O2 95.51(4) 100_655 . ?
O1 Cu1 Cu1 84.49(4) . 121_655 ?
O1 Cu1 Cu1 84.49(4) 115 121_655 ?
O1 Cu1 Cu1 84.49(4) 18_655 121_655 ?
O1 Cu1 Cu1 84.49(4) 100_655 121_655 ?
O2 Cu1 Cu1 180.00(8) . 121_655 ?
C1 O1 Cu1 122.59(13) . . ?
Cu1 O2 H1O2 134.1(17) . . ?
Cu1 O2 H1O2 134.1(17) . 18_655 ?
H1O2 O2 H1O2 92(3) . 18_655 ?
O1 C1 O1 125.7(2) 138 . ?
O1 C1 C2 117.11(11) 138 . ?
O1 C1 C2 117.11(11) . . ?
C3 C2 C3 120.2(2) . 30 ?
C3 C2 C1 119.83(12) . . ?
C3 C2 C1 119.83(12) 30 . ?
C2 C3 C2 119.8(2) 84 . ?
C2 C3 H3 120.1 84 . ?
C2 C3 H3 120.1 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
Cu1 O1 C1 O1 3.9(4) . . . 138 ?
Cu1 O1 C1 C2 -173.64(14) . . . . ?
O1 C1 C2 C3 -176.8(2) 138 . . . ?
O1 C1 C2 C3 0.9(3) . . . . ?
O1 C1 C2 C3 -0.9(3) 138 . . 30 ?
O1 C1 C2 C3 176.8(2) . . . 30 ?
C3 C2 C3 C2 -0.8(5) 30 . . 84 ?
C1 C2 C3 C2 175.10(16) . . . 84 ?
 
_refine_diff_density_max    0.813
_refine_diff_density_min   -0.439
_refine_diff_density_rms    0.072




# start Validation Reply Form
_vrf_PLAT420_Pristine-HK
;
PROBLEM: D-H Without Acceptor       O2       --H1O2     .     Please Check 
RESPONSE: The solvent is removed through the SQUEEZE in the software of Platon 
and there is no molecule that can hydrogen bond around H1O2.
;
# end Validation Reply Form



















