Metathesis in Single Crystal: Complete and Reversible Exchange of Metal Ions Constituting the Frameworks of Metal-Organic Frameworks
Sunirban Das; Hyunuk Kim; Kimoon Kim; Journal of the American Chemical Society 131 (2009) 3814–3815; doi:10.1021/ja808995d

data_4104064
_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 O51 Pb12'
_chemical_formula_sum            'C336 H312 O51 Pb12'
_chemical_formula_weight         7652.16
_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                   48.793(6)
_cell_length_b                   48.793(6)
_cell_length_c                   48.793(6)
_cell_measurement_reflns_used    3208
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.27
_cell_measurement_theta_min      2.11
_cell_volume                     116164(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      298(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'ADSC Quantum 210'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_source         'PAL 4A MXW Beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.90001
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0130
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            55468
_diffrn_reflns_theta_full        29.27
_diffrn_reflns_theta_max         29.27
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    4.044
_exptl_absorpt_correction_T_max  0.7934
_exptl_absorpt_correction_T_min  0.6879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.875
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             29760
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.335
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.000029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+1205.5813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1938
_reflns_number_gt                2572
_reflns_number_total             3208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808995d_si_002_11.cif
_cod_data_source_block           1-12h
_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 O4.25 Pb'
_cod_original_formula_weight         637.68
_cod_original_formula_moiety         'C28 H26 O4.25 Pb'
_cod_original_formula_units_Z            96
_cod_original_cell_volume        116163(23)
_cod_database_code               4104064