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_4346070
_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 (C12 H12 O4)4], 4H2 O'
_chemical_formula_sum            'C48 H56 O20 Pb4'
_chemical_formula_weight         1781.68
_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                   20.9045(4)
_cell_length_b                   20.9045
_cell_length_c                   8.1317(3)
_cell_measurement_reflns_used    6290
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.1600
_cell_measurement_theta_min      2.6630
_cell_volume                     3553.54(15)
_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 0.997
_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  0.0491
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18702
_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         27.562
_diffrn_reflns_theta_min         2.756
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.502
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2014)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       prism
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.128
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details '1892 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.013(8)
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         4098
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0393P)^2^+0.7969P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                3711
_reflns_number_total             4098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00185_si_002.cif
_cod_data_source_block           2
_cod_database_code               4346070
_shelx_estimated_absorpt_t_min   0.163
_shelx_estimated_absorpt_t_max   0.252