Supramolecular Porous Assemblies of Atomically Precise Catalytically Active Cerium-Based Clusters
Wasson, Megan C.; Zhang, Xuan; Otake, Ken-ichi; Rosen, Andrew S.; Alayoglu, Selim; Krzyaniak, Matthew D.; Chen, Zhijie; Redfern, Louis R.; Robison, Lee; Son, Florencia A.; Chen, Yongwei; Islamoglu, Timur; Notestein, Justin M.; Snurr, Randall Q.; Wasielewski, Michael R.; Farha, Omar K.; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c02740

data_4003685
_publ_section_title
;
 Supramolecular Porous Assemblies of Atomically Precise Catalytically
 Active Cerium-Based Clusters
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c02740
_journal_year                    2020
_chemical_formula_moiety         'Ce38 O33.33'
_chemical_formula_sum            'Ce38 O33.33'
_chemical_formula_weight         5857.92
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_primary     direct
_audit_creation_date             2020-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.1726(18)
_cell_length_b                   25.1726(18)
_cell_length_c                   36.760(3)
_cell_measurement_reflns_used    9415
_cell_measurement_temperature    250
_cell_measurement_theta_max      36.47
_cell_measurement_theta_min      2.48
_cell_volume                     23293(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      250.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.265
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.265
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22059
_diffrn_reflns_point_group_measured_fraction_full 0.265
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         36.499
_diffrn_reflns_theta_min         2.482
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    28.049
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.5531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1448 before and 0.0715 after correction. The Ratio of minimum to maximum transmission is 0.7402. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.835
_exptl_crystal_description       block
_exptl_crystal_F_000             4941
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.945
_refine_diff_density_min         -2.823
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.644
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         5596
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      3.710
_refine_ls_R_factor_all          0.4172
_refine_ls_R_factor_gt           0.3723
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.7872
_refine_ls_wR_factor_ref         0.8067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3301
_reflns_number_total             5596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c02740_si_003.cif
_cod_data_source_block           13119ce38na_1_149_2_0m
_cod_original_cell_volume        23293(4)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4003685
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.604
_olex2_refinement_description
;
1. Restrained distances
 Ce8_$1-O8_$1 \\sim Ce2_$2-O8_$1 \\sim Ce9_$1-O8_$1
 with sigma of 0.02
 Ce5-O10_$1 \\sim Ce10-O10_$1 \\sim Ce9_$1-O10_$1 \\sim Ce6-O10_$1
 with sigma of 0.02
 Ce4_$2-O1_$2 \\sim Ce3_$2-O1_$2
 with sigma of 0.02
 Ce3-O6 \\sim Ce8-O6
 with sigma of 0.02
 Ce1-O4 \\sim Ce6-O4 \\sim Ce4-O4 \\sim Ce7-O4
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uiso(O8) = Uiso(O9) = Uiso(O5) = Uiso(O4) = Uiso(O10) = Uiso(O6)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O8(0.33333)
;
_olex2_submission_special_instructions 'No special instructions were received'