Robust molecular bowl-based metal-organic frameworks with open metal sites: size modulation to increase the catalytic activity.
Liu, Lin; Han, Zheng-Bo; Wang, Shi-Ming; Yuan, Da-Qiang; Ng, Seik Weng; Inorganic chemistry 54 (2015) 3719–3721; doi:10.1021/acs.inorgchem.5b00185

data_4346069
_publ_section_title
;
 Robust molecular bowl-based metal-organic frameworks with open metal
 sites: size modulation to increase the catalytic activity.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3719
_journal_page_last               3721
_journal_paper_doi               10.1021/acs.inorgchem.5b00185
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '[Pb4 (C3 H7 N O) (C12 H12 O4)4], 0.5(H2 O)'
_chemical_formula_sum            'C60 H77 N4 O20.5 Pb4'
_chemical_formula_weight         2011.01
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.7139(3)
_cell_length_b                   20.7139
_cell_length_c                   8.1430(2)
_cell_measurement_reflns_used    4960
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4760
_cell_measurement_theta_min      2.6650
_cell_volume                     3493.88(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12531
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         2.781
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2014)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       prism
_exptl_crystal_F_000             1914
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
 The Pb1 atom is disordered over two positions in a nearly 1:1 ratio.  

The formula was established on the basis of C&H elemental analysis to consists
of one tetranuclear molecule and four water molecules.  Because of the disorder
in the heavy atom, the water molecule is also probably disordered in the same
ratio.  

When only normal Pb--O bonds are considered, the Pb1 and Pb1' atoms are 
four-coordinate; the lone-pair of electrons is stereochemically active.

The electron density of the 4 water molecules in each of the two Wyckoff 2a 
sites were treated by the SQUEEZE option in PLATON.
;
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details '1859 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         4027
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+3.2015P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0537
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                3651
_reflns_number_total             4027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00185_si_002.cif
_cod_data_source_block           1
_cod_database_code               4346069
_shelx_estimated_absorpt_t_min   0.159
_shelx_estimated_absorpt_t_max   0.643