#------------------------------------------------------------------------------
#$Date: 2021-08-30 09:29:47 +0300 (Mon, 30 Aug 2021) $
#$Revision: 268283 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/40/4104056.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_4104056
loop_
_publ_author_name
'Sunirban Das'
'Hyunuk Kim'
'Kimoon Kim'
_publ_section_title
;
 Metathesis in Single Crystal: Complete and Reversible Exchange of Metal
 Ions Constituting the Frameworks of Metal-Organic Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3814
_journal_page_last               3815
_journal_paper_doi               10.1021/ja808995d
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C336 H312 O63 Pb12, 156O'
_chemical_formula_sum            'C336 H312 O219 Pb12'
_chemical_formula_weight         10340.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           226
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4a 2 3'
_symmetry_space_group_name_H-M   'F m -3 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   48.850(6)
_cell_length_b                   48.850(6)
_cell_length_c                   48.850(6)
_cell_measurement_reflns_used    4722
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      2.10
_cell_volume                     116572(2)
_computing_cell_refinement       'DENZO (Z. Otwinowski and W. Minor, 1997)'
_computing_data_collection       'ADSC Quantum software'
_computing_data_reduction        'HKL2000 (Z. Otwinowski and W. Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'ADSC Quantum 210'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_source         'PAL 4A MXW Beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            95172
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    4.122
_exptl_absorpt_correction_T_max  0.4781
_exptl_absorpt_correction_T_min  0.3915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             40512
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.963
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0917P)²+1192.7052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                4545
_reflns_number_total             4722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808995d_si_002_03.cif
_cod_data_source_block           2
_cod_depositor_comments
;

2021-08-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C28 H26 O18.25 Pb'
_cod_original_formula_weight         861.68
_cod_original_formula_moiety         'C28 H26 O5.25 Pb, 13O'
_cod_original_formula_units_Z            96
_cod_original_cell_volume        116575(23)
_cod_database_code               4104056
loop_
_symmetry_equiv_pos_as_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+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+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, -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+1/2, x+1, -z+1'
'-y+1/2, -x+1, -z+1'
'y+1/2, -x+1, z+1'
'-y+1/2, x+1, z+1'
'x+1/2, z+1, -y+1'
'-x+1/2, z+1, y+1'
'-x+1/2, -z+1, -y+1'
'x+1/2, -z+1, y+1'
'z+1/2, y+1, -x+1'
'z+1/2, -y+1, x+1'
'-z+1/2, y+1, x+1'
'-z+1/2, -y+1, -x+1'
'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, x+1/2, -z+1'
'-y+1, -x+1/2, -z+1'
'y+1, -x+1/2, z+1'
'-y+1, x+1/2, z+1'
'x+1, z+1/2, -y+1'
'-x+1, z+1/2, y+1'
'-x+1, -z+1/2, -y+1'
'x+1, -z+1/2, y+1'
'z+1, y+1/2, -x+1'
'z+1, -y+1/2, x+1'
'-z+1, y+1/2, x+1'
'-z+1, -y+1/2, -x+1'
'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, x+1, -z+1/2'
'-y+1, -x+1, -z+1/2'
'y+1, -x+1, z+1/2'
'-y+1, x+1, z+1/2'
'x+1, z+1, -y+1/2'
'-x+1, z+1, y+1/2'
'-x+1, -z+1, -y+1/2'
'x+1, -z+1, y+1/2'
'z+1, y+1, -x+1/2'
'z+1, -y+1, x+1/2'
'-z+1, y+1, x+1/2'
'-z+1, -y+1, -x+1/2'
'-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-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'y-1/2, -x-1/2, -z-1/2'
'-x-1/2, -z-1/2, y-1/2'
'x-1/2, -z-1/2, -y-1/2'
'x-1/2, z-1/2, y-1/2'
'-x-1/2, z-1/2, -y-1/2'
'-z-1/2, -y-1/2, x-1/2'
'-z-1/2, y-1/2, -x-1/2'
'z-1/2, -y-1/2, -x-1/2'
'z-1/2, y-1/2, x-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, 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-1/2, -x, z'
'y-1/2, x, z'
'-y-1/2, x, -z'
'y-1/2, -x, -z'
'-x-1/2, -z, y'
'x-1/2, -z, -y'
'x-1/2, z, y'
'-x-1/2, z, -y'
'-z-1/2, -y, x'
'-z-1/2, y, -x'
'z-1/2, -y, -x'
'z-1/2, y, x'
'-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, -x-1/2, z'
'y, x-1/2, z'
'-y, x-1/2, -z'
'y, -x-1/2, -z'
'-x, -z-1/2, y'
'x, -z-1/2, -y'
'x, z-1/2, y'
'-x, z-1/2, -y'
'-z, -y-1/2, x'
'-z, y-1/2, -x'
'z, -y-1/2, -x'
'z, y-1/2, x'
'-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, -x, z-1/2'
'y, x, z-1/2'
'-y, x, -z-1/2'
'y, -x, -z-1/2'
'-x, -z, y-1/2'
'x, -z, -y-1/2'
'x, z, y-1/2'
'-x, z, -y-1/2'
'-z, -y, x-1/2'
'-z, y, -x-1/2'
'z, -y, -x-1/2'
'z, y, x-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pb1 Pb 0.220953(7) 0.0000 0.194421(9) 0.0736(2) Uani 1 2 d S
O1 O 0.26146(10) -0.03170(10) 0.19912(11) 0.0871(14) Uani 1 1 d .
O2 O 0.23934(9) -0.03289(8) 0.16079(10) 0.0724(11) Uani 1 1 d .
O3 O 0.2500 0.0000 0.2500 0.063(2) Uani 1 8 d S
O1W O 0.18213(19) 0.0000 0.1579(3) 0.153(4) Uani 1 2 d S
C1 C 0.25829(11) -0.04120(10) 0.17535(13) 0.0596(13) Uani 1 1 d .
C2 C 0.27646(10) -0.06377(10) 0.16607(12) 0.0555(12) Uani 1 1 d .
C3 C 0.29882(11) -0.07185(10) 0.18166(13) 0.0595(13) Uani 1 1 d .
H3 H 0.3029 -0.0628 0.1984 0.071 Uiso 1 1 calc R
C4 C 0.31524(11) -0.09318(10) 0.17260(12) 0.0569(12) Uani 1 1 d .
C5 C 0.30922(10) -0.10744(10) 0.14864(11) 0.0549(12) Uani 1 1 d .
C6 C 0.28691(11) -0.09892(11) 0.13287(12) 0.0608(13) Uani 1 1 d .
H6 H 0.2826 -0.1081 0.1163 0.073 Uiso 1 1 calc R
C7 C 0.27112(11) -0.07712(11) 0.14151(12) 0.0599(13) Uani 1 1 d .
H7 H 0.2563 -0.0711 0.1304 0.072 Uiso 1 1 calc R
C8 C 0.34071(12) -0.10358(12) 0.18660(12) 0.0618(13) Uani 1 1 d .
C9 C 0.34900(11) -0.12693(10) 0.16740(11) 0.0569(12) Uani 1 1 d .
C10 C 0.32994(11) -0.12969(11) 0.14563(11) 0.0542(12) Uani 1 1 d .
C11 C 0.33322(14) -0.11386(13) 0.21558(13) 0.0730(16) Uani 1 1 d .
H11A H 0.3502 -0.1199 0.2248 0.088 Uiso 1 1 calc R
H11B H 0.3257 -0.0983 0.2262 0.088 Uiso 1 1 calc R
C12 C 0.31257(19) -0.13729(19) 0.21636(16) 0.095(2) Uani 1 1 d .
H12A H 0.2970 -0.1329 0.2045 0.143 Uiso 1 1 calc R
H12B H 0.3061 -0.1399 0.2352 0.143 Uiso 1 1 calc R
H12C H 0.3213 -0.1541 0.2099 0.143 Uiso 1 1 calc R
C13 C 0.36188(13) -0.08002(12) 0.18718(15) 0.0711(16) Uani 1 1 d .
H13A H 0.3546 -0.0650 0.1987 0.085 Uiso 1 1 calc R
H13B H 0.3789 -0.0868 0.1959 0.085 Uiso 1 1 calc R
C14 C 0.36886(19) -0.0686(2) 0.1595(2) 0.103(3) Uani 1 1 d .
H14A H 0.3777 -0.0829 0.1485 0.154 Uiso 1 1 calc R
H14B H 0.3813 -0.0531 0.1616 0.154 Uiso 1 1 calc R
H14C H 0.3521 -0.0626 0.1504 0.154 Uiso 1 1 calc R
O2W O 0.1271(4) 0.0141(4) 0.1736(4) 0.304(9) Uiso 1 1 d .
O3W O 0.3244(4) -0.0588(4) 0.0980(4) 0.303(9) Uiso 1 1 d .
O4W O 0.2500 -0.0740(4) 0.0740(4) 0.289(10) Uiso 1 2 d S
O5W O 0.2333(3) -0.0254(3) 0.1052(3) 0.249(6) Uiso 1 1 d .
O6W O 0.4312(4) -0.0553(4) 0.2069(4) 0.294(8) Uiso 1 1 d .
O7W O 0.4003(7) 0.0000 0.1908(7) 0.315(13) Uiso 1 2 d S
O8W O 0.2773(7) 0.0000 0.1146(7) 0.348(16) Uiso 1 2 d S
O9W O 0.4182(8) 0.0000 0.1366(8) 0.351(16) Uiso 1 2 d S
O10W O 0.1066(9) 0.0000 0.1281(9) 0.43(2) Uiso 1 2 d S
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 0.0021 '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 -0.0042 0.0079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -7.7823 10.5819 '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 Pb1 O2 81.3(2) . 99
O2 Pb1 O1 51.34(15) . .
O2 Pb1 O1 100.05(18) 99 .
O2 Pb1 O1 100.06(18) . 99
O2 Pb1 O1 51.35(15) 99 99
O1 Pb1 O1 75.7(2) . 99
O2 Pb1 O1W 79.0(2) . .
O2 Pb1 O1W 79.0(2) 99 .
O1 Pb1 O1W 129.3(2) . .
O1 Pb1 O1W 129.3(2) 99 .
C1 O1 Pb1 92.6(3) . .
C1 O2 Pb1 95.9(4) . .
O2 C1 O1 120.1(5) . .
O2 C1 C2 121.0(5) . .
O1 C1 C2 118.7(5) . .
C3 C2 C7 119.2(5) . .
C3 C2 C1 120.9(5) . .
C7 C2 C1 119.9(5) . .
C4 C3 C2 119.5(5) . .
C3 C4 C5 121.4(5) . .
C3 C4 C8 125.8(5) . .
C5 C4 C8 112.8(4) . .
C4 C5 C6 118.6(5) . .
C4 C5 C10 107.7(4) . .
C6 C5 C10 133.7(5) . .
C7 C6 C5 119.8(5) . .
C6 C7 C2 121.4(5) . .
C4 C8 C9 101.0(4) . .
C4 C8 C11 109.2(5) . .
C9 C8 C11 112.4(5) . .
C4 C8 C13 108.0(5) . .
C9 C8 C13 112.9(5) . .
C11 C8 C13 112.5(5) . .
C10 C9 C10 119.9(5) 59 .
C10 C9 C8 129.0(5) 59 .
C10 C9 C8 110.9(4) . .
C9 C10 C9 120.1(5) 80_545 .
C9 C10 C5 132.3(5) 80_545 .
C9 C10 C5 107.6(4) . .
C12 C11 C8 115.0(5) . .
C14 C13 C8 114.2(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O2 2.467(4) .
Pb1 O2 2.467(4) 99
Pb1 O1 2.523(4) .
Pb1 O1 2.523(4) 99
Pb1 O1W 2.603(11) .
O1 C1 1.260(7) .
O2 C1 1.236(7) .
C1 C2 1.486(7) .
C2 C3 1.389(8) .
C2 C7 1.390(8) .
C3 C4 1.387(7) .
C4 C5 1.394(7) .
C4 C8 1.508(7) .
C5 C6 1.398(7) .
C5 C10 1.493(7) .
C6 C7 1.381(8) .
C8 C9 1.532(7) .
C8 C11 1.546(9) .
C8 C13 1.548(9) .
C9 C10 1.391(7) 59
C9 C10 1.420(7) .
C10 C9 1.391(7) 80_545
C11 C12 1.526(11) .
C13 C14 1.500(12) .
O2W O2W 1.38(4) 99
